LOSS ON IGNITION: ESTIMATION OF SOIL ORGANIC

CARBON CONTENT IN SOILS OF KASHMIR

Introduction:

The word soil is derived through Old French from the Latin solum, which
means ground. It is defined as unconsolidated mineral matter on the surface of
earth that has been subjected to and influenced by genetic and environmental
factors of parent material, climate, micro and macroorganisms, and
topography, all acting over a period of time and producing a product called
Soil that differs from the material from which it has been derived in many
physical, chemical and biological properties and characteristics (Soil Science
Society of America, 2008). Engineers might define soil by saying that it
occupies the unconsolidated mantle of weathered rocks making up the loose
materials on the Earth’s surface, commonly known as the regolith. Soil can be
described as a three-phase system, composed of a solid, liquid and gaseous
phase which in simple words, soil can be defined as the topmost layer of
decomposed rocks and organic matter usually containing air, moisture and
nutrients and therefore can support.
Soil consists of a finely divided layer of weathered minerals and organic matter
upon which plants grow and is the most fundamental requirement for
agriculture. To humans and most terrestrial organisms, soil is the most
important part of the geosphere. Though only a tissue thin layer compared to
the earth’s total diameter, soil is the medium that produces most of food
required by most living things. Good soil and a climate conducive to its
productivity is the most valuable asset a nation can have. In addition to this,
soil is the receptor of large quantities of pollutants, such as particulate matter
from power plant smokestacks. Fertilizers, pesticides, and some other materials
applied to soil often contribute to water and air pollution. Therefore, soil is a
key component of environmental chemical cycles.
Soils are formed by the weathering of parent rocks as a result of interactive
geological, hydrological and biological processes. Soils are porous and
vertically stratified into horizons as a result of downward percolating water
and biological processes, including the production and decay of biomass. Soils
are open systems that undergo continual exchange of matter and energy with
the atmosphere, hydrosphere and biosphere. Soils play a variety of roles in the
systems which are important to us. Soil is a medium for plant growth as it
provides vital resources and performs essential functions for the plants. It
provides pore spaces for roots to grow and also provides the air spaces which
act as a ventilation system for the plants. It also regulates the temperature
fluctuations and regulates water supply for the sustainable growth of plants.
The soaked water is retained in soil pores which is then used up by plants. Soil
is a habitat for many soil organisms and is also a source of minerals valuable
for many puposes. It recycles raw materials and is probably premier recycler
on earth. Soil possesses incomparable ability and capacity to assimilate great
quantities of organic wastes, turns the beneficial organic matter (humus) and
then converts the nutrients in the wastes to forms that can be utilized by plants
and animals. Soils have the capacity to accumulate large amounts of carbon as
soil organic matter, which can have a major impact on global changes such as
greenhouse effect.
Soil composition
Soil is not simply one thing but actually made up of several components and a
variable mixture of minerals, organic matter and water capable of supporting
plant life on the earth’s surface. The soil is in fact a three-phase system of
solid, liquid and gaseous components, each of which has its own physical and
chemical properties in an equilibrium or transient state, in relation to others.
Water, a part of the three phase, solid-liquid-gas system makes up soil and is a
basic transport medium for carrying essential plant nutrients from solid soil
particles into plant roots. Soils high in organic matter may hold appreciably
more water than other soils, but is relatively less available to plants because of
physical and chemical sorption of water by organic matter. The spaces in
between mineral particles as well as between aggregates of soil are occupied
by the gases which make the atmosphere of soil. Soil aeration is influenced by
pore spaces present in different numbers and sizes in different textures of soil.
Gases present in these pore spaces are more or less similar to those found in
external atmosphere. However, oxygen concentration is less and that of CO 2
higher in soil than those in atmosphere. The organic portion of soil consists of
plant biomass in various stages of decay. The soil fraction of typical
productive soil is approximately 5% organic matter and 95% inorganic matter.
Some soils, such as peat soils, may contain as much as 95% organic material.
Other soils contain as little as 1% organic matter. The organic matter in the soil
largely determines soil productivity and serves as a source of food for micro-
organisms, undergoes chemical reactions such as ion exchange and influences
the physical properties of soil. Some organic compounds even contribute to the
weathering of mineral matter, the process by which soil is formed. The
inorganic components of soil are formed from the weathering of parent rocks
and minerals which ultimately result in the formation of inorganic colloids,
which are the repositories of water and plant nutrients. Subsequently made
available to plants as needed. These colloids often absorb toxic substances in
soil. As a result of varying degrees of weathering of parent material, the
mineral particles of different sizes are formed. In a given sample of soil, there
may be present, different sized particles in different proportions which
determines the soil texture and hence directly influences soil-water
relationship, aeration and root penetration through its relationship interparticle
pore space. In addition to these components, each soil has a distinctive flora
and fauna of bacteria, fungi, algae, blue-green algae, protozoa, rotifers,
nematodes, oligochaetes, molluscs, arthropods etc which form the biotic
component of the soil.
Soil Organic Carbon
Soil organic carbon which is present as soil organic matter, it includes
relatively available C as fresh plant remains and relatively inert C in materials
derived from plant remains: humus and charcoal. Soil organic carbon is
divided between living soil biota and dead biotic material derived from
biomass. Together these comprise the soil food web, with the living
component sustained by the biotic material component. Soil biota includes
earthworms, nematodes, protozoa, fungi, bacteria and different arthropods.
Detritus resulting from plant senescence is the major source of soil organic
carbon. Plant materials, with cell walls high in cellulose and lignin, are
decomposed and the non-respired carbon is retained as humus. Cellulose and
starches are easily degraded, resulting in relatively short residence times. More
persistent forms of organic C include lignin, humus, organic matter
encapsulated in soil aggregates, and charcoal. Soil organic carbon tends to be
concentrated in the topsoil which ranges from 0.5% to 3.0% organic C for
most upland soils. Soils with less than 0.5% organic C are mostly limited to
desert areas. Soils containing greater than 12 - 18% organic C are generally
classified as organic soils. High levels of organic C develop in soils supporting
wetland ecology, flood deposition, fire ecology, and human activity. Fire
derived forms of carbon are present in most soils as unweathered charcoal and
weathered black carbon. Soil organic C is typically 5 - 50% derived from char,
with levels above 50% encountered in mollisol, chernozem, and terra preta
soils. Root exudates are another source of soil carbon, 5 - 20% of the total
plant carbon fixed during photosynthesis is supplied as root exudates in
support of rhizospheric mutualistic biota. Microbial populations are typically
higher in the rhizosphere than in adjacent bulk soil. SOC is a very important
component of the global carbon cycle, and the fate of SOC will have an
important impact on the future global climate. Soil organic carbon is a major
component of the global C budget, with the estimated 1500 Gt representing
more than the combined stocks of the atmosphere and biosphere (Eswaran et
al., 2000; Lal, 2004). There is now a widespread recognition that maximizing
storage of carbon in our soils offers a potentially crucial avenue to offset
increasing atmospheric carbon levels and thereby help in mitigating the effects
of human induced climate change (Lal et al., 2007; Smith, 2012; IPCC, 2014).
The association of SOC with soil health and agricultural productivity provides
an added incentive to promote soil carbon levels (Baldock et al., 2009;
Sanderman et al., 2010). The potential importance of soil carbon to humankind
was expressed by Lal (2004), as the close link between soil carbon
sequestration and world food security on the one hand and climate change on
the other can neither be overemphasized nor ignored. The SOC pool stores an
estimated 1500 PgC in the first meter of soil, which is more carbon than is
contained in the atmosphere (roughly 800 PgC) and terrestrial vegetation (500
Pg C) combined (FAO and ITPS, 2015). This phenomenal SOC reservoir is not
static, but is constantly cycling between the different global carbon pools in
various molecular forms (Kane, 2015). This organic material transformation
process results in a complex biogeochemical mixture of plant litter compounds
and microbial decomposition products in various stages of decomposition
(Von Lützow et al., 2006; Paul, 2014) that can be associated with soil minerals
and occluded within aggregates, enabling SOC persistence in soil for decades,
centuries or even millennia (Schmidt et al., 2011). CO 2 is emitted back into the
atmosphere when soil organic matter (SOM) is decomposed (or mineralized)
by microorganisms. Carbon loss can also be caused by root exudates such as
oxalic acid, which liberate organic compounds from protective mineral
associations (Keiluweit et al., 2015). Finally, carbon is also partly exported
from soils to rivers and oceans as dissolved organic carbon (DOC) or as part of
erosion material. In principle, the amount of SOC stored in a given soil is
dependent on the equilibrium between the amount of carbon entering the soil
and the amount of carbon leaving the soil as carbon-based respiration gases
resulting from microbial mineralization and, to a lesser extent, leaching from
the soil as DOC. Locally, C can also be lost or gained through soil erosion or
deposition, leading to the redistribution of soil C at local, landscape and
regional scales. Levels of SOC storage are therefore mainly controlled by
managing the amount and type of organic residues that enter the soil and
minimizing the soil carbon losses (FAO and ITPS, 2015). The quantification of
global carbon fluxes is necessary to clarify, amongst others, whether global
terrestrial ecosystems fix more atmospheric CO 2 via photosynthesis than they
return to the atmosphere through respiration. SOM contains roughly 55–60%
carbon by mass. In many soils, this carbon comprises most or all of the carbon
stock – referred to as SOC – except where inorganic forms of soil carbon occur
(FAO and ITPS, 2015). Similar to SOM, SOC is divided into different pools as
a function of its physical and chemical stability (FAO and ITPS, 2015;
O’Rourke et al., 2015). Fast pool (labile or active pool) - After addition of
fresh organic carbon to the soil, decomposition results in a large proportion of
the initial biomass being lost in 1–2 years. Intermediate pool - Comprises
microbially processed organic carbon that is partially stabilized on mineral
surfaces and/or protected within aggregates, with turnover times in the range of
10-100 years. Slow pool (refractory or stable pool) - highly stabilized SOC,
enters a period of very slow turnover of 100 to 1000 years. An additional slow
SOC pool is pyrogenic SOC, formed from partially carbonized biomass during
wildfires (Schmidt and Noack, 2000) which is present in many ecosystems. A
portion of this material has a highly condensed aromatic chemical structure
(often referred to as pyrogenic carbon or black carbon) that resists microbial
degradation and thus persists in soils for longer periods (Lehmann et al., 2015).
The separation of SOC into different pools is largely more conceptual than
measurable and is based on the ease of SOC oxidation or degree of physical
stabilization within aggregates or through attachment to minerals determined
through analytical protocols. Although SOC pools are often used to model
carbon dynamics, ways to reconcile “measurable” and “modellable” pools
have rarely been reported (Zimmermann et al., 2007; Luo et al., 2014). This
Soil organic carbon is stored in the soil by a process called Carbon
sequestration in which carbon is fixed from the atmosphere via plants or
organic residues and stored in the soil. When dealing with CO 2, SOC
sequestration involves three stages:
1) the removal of CO2 from the atmosphere via plant photosynthesis;

2) the transfer of carbon from CO2 to plant biomass; and

3) the transfer of carbon from plant biomass to the soil where it is stored in the
form of SOC in the most labile pool.
This pool is characterized by the highest turnover rate (days - few years),
encompasses recently incorporated plant residues and is readily decomposable
by soil fauna, generally causing CO2 emissions back into the atmosphere.

Importance of Organic Carbon in soil:

The importance of soil organic carbon for positive environmental and
development outcomes has gained recognition as a result of breakthrough
decisions at the twelfth session of the Conference of Parties (COP) of the
United Nations Convention to Combat Desertification (UNCCD) in October
2015. Soil organic carbon is recognised as a major determinant of agricultural
productivity and water security, and it is the cornerstone of biodiversity and
climate change resilience. There are many production and environmental
benefits associated with increasing SOC which include improved soil structure,
increased soil fertility, increased water holding capacity, increased water use
efficiency, increased biological activity, increased plant growth and yields,
increased resilience to dry periods and reduced erosion risk. Recent studies
assessing SOC sequestration and C emissions in intensively managed
agricultural lands where the value of SOC is often linked to climate change
mitigation. This is not, however, the only reason for promoting C storage in the
soil. It is important to remember that SOC plays a critical role in improving
physical, chemical, and biological processes and properties. SOC is both a
source of nutrients and mechanism for nutrient retention, it affects water
infiltration as well as increases retention of plant available water and it
provides favourable conditions for soil biota (Piéri,1985, Bationo and
Mokwunye, 1991; Kablan et al., 2009; Konare et al., 2010). Some of the soil
processes influenced by SOC include aggregation, compaction, energy fluxes
(water, gas, and air), surface sealing, crusting, and cracking, water and wind
erosion, wetting–drying cycles, shrink–swell potential, microbial activity,
biodegradation of pollutants, and others. While the agricultural sector has the
ability to impact the carbon cycle on a large scale, often through the release of
carbon, farmer shave a vested interest in retaining and increasing soil organic
carbon for individual fields because soil and yield tend to improve when the
soil organic carbon level increases. Higher soil organic carbon promotes soil
structure or tilth meaning there is greater physical stability. This improves soil
aeration (oxygen in the soil) and water drainage and retention, and reduces the
risk of erosion and nutrient leaching. Soil organic carbon is also important to
chemical composition and biological productivity, including fertility and
nutrient holding capacity of a field (FAO and ITPS 2015, SWSR). As carbon
stores in the soil increase, carbon is “sequestered”, and the risk of loss of other
nutrients through erosion and leaching is reduced. An increase in soil organic
carbon typically results in a more stable carbon cycle and enhanced overall
agricultural productivity, while physical disturbances of the soil can lead to a
net loss of carbon into the surrounding environment due to formation of carbon
dioxide (CO2).
Improvement in one soil property by SOC concomitantly affects other
properties and processes as the physical, chemical, and biological properties
are all interrelated e.g., an increase in soil aggregate stability can enhance
macro porosity, water infiltration, and soil microbial activity. There is a mutual
relationship between SOC and soil properties as for instance, SOC improves
aggregation, and in turn, stable aggregates protect and promote long-term SOC
storage. The magnitude of SOC effects on soil properties can vary with clay
content and mineralogy, soil Carbon pool components (labile and stable
Carbon), and climate among others (Lal, 2013). For example, an increase in
SOC may have more beneficial effects on silt loams than on clayey soils.
Because the organic and clay mineral fraction have some similar properties
(i.e., high specific surface area), high clay concentration may reduce the
benefits from increased SOC. These factors deserve consideration when
quantifying the SOC effects on soil properties.
Soil organic carbon (SOC), is vital to essential soil functions and to the
ecosystem services. Farming practices cause declining returns and inputs of
carbon (C) to soils and pose threats to soil functions, but a number of farming
practices have shown potential for increasing SOC content and can contribute
to improve long-term crop productivity, improve the physical and biological
properties and carbon sequestration (Blanco-Canqui et al., 2013). The global
importance of dry lands for storage of soil organic carbon may not be apparent.
The scarcity of water in dry lands constrains plant productivity, which affects
SOM and SOC accumulation in soils. As a result, dry land soils typically have
low organic carbon content, often less than 1% of the soil mass. In grassland or
forest soils SOC may be as high as 4-5% but cultivation of the soil acts to
release its stored carbon; in temperate zones SOC is around 1-2% in cultivated
soils (Le Quéré et al. 2016; Scharlemann et al. 2014). Due to their vast extent,
the total stock of accumulated SOC in dry lands is significant, accounting for
around 30% of the global total SOC stocks, i.e. roughly 450 Gt C or about as
much as the organic carbon stocked in all terrestrial vegetation. Furthermore,
the residence time of carbon in dry land soils is extended due to their aridity
and is much longer than in other soils. The loss of organic carbon from soils,
especially when initial levels are low as is the case in dry land regions,
invariably results in the degradation of soils and their associated ecosystem
functions. Between one quarter and one third of all land worldwide is
estimated to be affected by some form of land degradation, that is contributing
to declines in agricultural production, disruption of water cycles, release of
greenhouse gasses, and many other costs to society. These negative impacts
have to be seen in a perspective where the human population is estimated to
require an additional 60% of food by the year 2050 and by 2025, 1.8 billion
people are projected to be living in areas with absolute water scarcity (Soil
Organic Carbon Fact Sheet, Agronomy Fact Sheet Series, Fact Sheet 91). Land
degradation and climate change could reduce agricultural yields and result in a
food production shortfall of 25% soil organic carbon are therefore an important
foundation of a broad range of ecosystem services across all four standard
ecosystem service categories.
Factors affecting Soil Organic Carbon
SOC levels are largely determined by three factors:
The amount of biomass grown – rainfall, soil fertility and crop type determine
the amount of plant biomass and hence the amount of organic material that can
be potentially returned to the soils.
Soil texture – clay provides protection from decomposition by microbes. The
higher the clay content, the higher the potential for soils to store organic
carbon.
Management – tillage of the soil reduces SOC by exposing it to organisms
breaking down organic materials. Grazing or burning of residues also reduces
the amount of organic material returned to the soils. Typically, pasture systems
tend to have higher SOC levels than cropping systems.
Beyond agronomic management, the direction and rate of change in SOC
content is also determined by many factors like the crop rotation patterns, input
rates of organic matter, chemical composition of organic matter inputs, soil
type and texture, the previous land use, the climatic conditions, the high
variability of SOC values between the sampling locations in the same field
which requires subsequent sampling to be repeated at the same spots over time
to eliminate any factor of spatial variability (Campbell et al., 1996; Larney et
al., 1997; Paustian et al., 1997; Balesdent et al., 2000).
Soil carbon levels are determined by factors such as rainfall, temperature,
vegetation and soil type and reach equilibrium values associated with
individual systems and locations. However, these equilibria are disturbed when
areas are cleared and used for agricultural production. Globally, clearing
natural vegetation for agriculture results in some large reductions in SOC
levels and further declines may occur due to management practices. In
agricultural systems, soil carbon levels tend to be variable and dependent on
management practices. The change in SOC is determined by the balance of
carbon inputs over losses.
Some management practices, such as fallowing, cultivation, stubble burning or
removal, and overgrazing can reduce SOC by reducing inputs to the soil,
increasing the decomposition of soil organic materials, or both. There are a
wide range of management options and farming practices that can increase
SOC levels by either increasing inputs or decreasing losses, e.g. stubble
retention. Inputs can also be increased by direct additions of organic materials,
composts, manure and other recycled organic materials. However, it should be
noted that some of the yield increasing practices involve the use of fertilisers
and irrigation water which require large energy consumption and therefore
increase carbon dioxide emission.
Long-term fate of active Carbon in forest ecosystems rely on whether it is
retained in living biomass or soils. World soils hold significant pool of active
Carbon that plays vital role in the global Carbon cycle (Prentice et al., 2001).
Soil carbon stock is greatly influenced by the type of forest, litter quality and
litter production by vegetation, soil properties and climate (Lal, 2001; Zhang et
al., 2013). Moreover, residence time of vegetation Carbon is less than that of
soil Carbon. Therefore, even a minute change in soil carbon pool could have
major impact on global atmospheric concentration (Medlyn et al., 2005).
Hence, it is pertinent to understand the variation in forest SOC and soil carbon
sequestration is considered to be viable option for reducing concentration of
atmospheric CO2 (Powlson et al., 2011).
Review of Literature

Lowther (1992) compared three methods of estimating soil organic carbon

(dichromate oxidation with and without external heating and loss on ignition)
with a method for total carbon measured in an automated resistance furnace in
38 surface podolized sands and observed that the concentration of total carbon
was highly correlated in all the three methods and ranged from 0.39 to 4.57%.
Jolivet et al (1998) collected samples from sandy soils of French Gascony
(spodosols) and compared results for analytical determination of organic
carbon (C) by wet and dry combustion of organic organic matter (OM) by loss-
on-ignition at 550°C. The results demonstrated that wet digestion
systematically underestimated Carbon content through Loss-on-ignition and
wet digestion measurements were well correlated to carbon content obtained
by dry combustion.
Konnen et al (2002) used the LOI method for predicting SOC in North Central
US soils by collecting nearly 255 samples and found that the organic carbon
concentration of samples ranged between 1.09 – 114.6 g/kg. In the same year
Bhatti and Bauer analyzed 307 samples of Peat and forest floor from sites
across continental western Canada to determine Carbon/Organic Matter ratio,
variability in C/OM ratio and influence of vegetation type and ash content on
C/OM ratio in which the results suggested that if LOI and organic C are
measured and equations are developed for a subset of samples, accurate
predictions of organic C can be made by using the LOI technique. Further
Loss-on-ignition provides a rapid, cost effective and simple technique for the
routine estimation of organic C for forest and peat land ecosystems.
Vos et al (2005) worked on checking the capability of LOI as predictor of
organic carbon in non-calcareous forest soils and observed that the highest
precision was found in floor samples (RSD<1.2%) and Lowest (5-10%) in
sandy soils samples.
Westman et al (2006) worked on LOI method for determining pools of
organic carbon in soils of Pristine forests and afforested arable fields and found
LOI as a good indicator of carbon concentration in organic layer. The results
also indicated that estimation of carbon pools from conversion factors would
lead to considerable bias and that direct measurement of Carbon concentration
is preferable to use of any Cc/LOI ratio.
Albela and Zimmer (2007) worked on estimating organic carbon from LOI in
Northern Arizona Forest soils taken from 102 plots by testing 9 LOI
temperature duration combinations 300°C to 600°C and 2-6 hours to discern
optimal combinations for estimating SOC. The values showed no consistent
trend to change with increasing duration, but tended to be slightly higher at the
lowest temperature (300°C). The results suggested that LOI may be useful for
roughly estimating SOC but other methods or modification to LOI are needed
when more accurate SOC measurements are required. Likewise, Kamara et al
(2007) carried out a study to estimate soil organic carbon using three different
methods, LOI, Walkley Black and Dry combustion and observed that both
temperature and sample weight had significant effects on LOI, but former had
greater effect with strong correlations between LOI and dry combustion carbon
for all aggregate size fractions.
Wright L et al (2008), worked on assessment of Soil organic Carbon in
Everglades Wetlands soils by LOI (Loss-on-ignition) on 3168 samples taken
from three soil depths in 14 wetlands and observed that the LOI was a better
predictor of total organic carbon when LOI exceeded 400 g/kg because of less
interference by CaCO3. The proportion of carbon in organic matter measured
by LOI method was more accurate and applicable across wetlands and soil
depths. In the same year Adolfo Campos analysed the relationship between
soil organic carbon content determined by dry combustion, Walkley-Black
method and loss-on-ignition (LOI) in soil samples collected from non-
calcareous O and A1 horizons within a tropical forest by developing linear
regression equations to estimate the organic carbon. The results showed that
LOI method produced a better linear relation with dry combustion than with
the Walkley-Black method. In another study conducted by Rawlins et al
(2008) for the estimation of SOC content in soils of urban areas of UK by LOI
analysis of 30 samples it was observed that LOI at 450°C accounts for a
consistent proportion of Black Carbon in each sample and LOI estimate of
SOC may be a cost-effective method for estimation of Black Carbon.
Szava-Kovats (2009) worked on relationship between organic carbon and LOI
in soil and the analysis of relationship between Organic Carbon and LOI
revealed that the relationship was non-linear.
Konare et al (2010) measured SOC in soils of Sahel West Africa in order to
provide a method which permit accurate assessment of SOC and observed that
the LOI method appeared to be useable for a range of soils collected in Mali by
being easier and more convenient than the expensive dry combustion method.
Rahman et al (2011) worked on estimation of carbon in 121 allophonic soil
samples of New Zealand, collected from 0-100 cm depth from three regions of
Kiwi fruit orchards. Many methods used to estimate SOC were found to be
relatively time consuming and costly, with carbon in soil samples converted to
carbon dioxide to be measured directly or indirectly by different methods. The
soil samples analysed using LOI to determine organic carbon by combination
of three different ignition temperatures and four-time durations revealed that
LOI method is well suited as a cost-effective method for analysis of SOC in
soils. Similarly, NKengfac et al (2011) carried out a study for estimating
organic carbon from loss-on-ignition and pH in some soils of Cameroon
Rubber plantations taken from (0-15cm) depth of the topsoil in mature Rubber
plantations in humid forests of southwest Cameroon. LOI-SOC-pH regression
equations obtained using data from analysis of topsoils in mature rubber
plantations again showed that LOI is a rapid, less costly and accurate method
for the estimating SOC. In the same year Wang et al (2011) worked on
optimizing the weight loss-on-ignition methodology to quantify organic and
carbonate carbon of sediments collected from canals, wetlands, rivers,
estuaries, lakes, and marine sites. Combinations of the combustion time and
temperature and optimal weight ranges of representative samples were tested
and comparisons of the WLOI method with other methods, including dry
combustion and wet combustion were made. The results of analysing samples
of sediments of diverse origins showed that the optimal combination of
temperature and time of WLOI depended mostly on the sources of the analysed
sediment. The WLOI analysis of sediment samples for organic Carbon from
wetlands, Canals, Estuaries or River sites needed a relatively low temperature
but that of sediment samples from lake and marine sites required a relatively
high temperature. It was concluded that WLOI, has advantages of simplicity,
cost-effectiveness and no waste disposal over other methods, besides providing
precise measurements of organic and inorganic Carbon contents in sediments
from a wide range of sources.
Ostrowska and Porębska (2012) analysed relations between the total organic
carbon (TOC) and the soil organic matter (SOM) in 47 soil profiles, dug out in
dry coniferous forests, fresh coniferous forests and mixed deciduous-
coniferous forests by using loss-on-ignition method. The results showed a
significant correlation between the content of TOC and SOM in all layers with
the regression coefficient of linear equations for the SOM to TOC conversion
decreasing with soil depth. In deeper layers, the relationship between TOC and
SOM seemed to be less evident.
Wang et al (2013) worked on LOI method to determine the SOC and SIC in
Arid Soils of North-western China at a combustion temperature of 375°C and
showed that there were strong linear relationship for both SOC and SIC
between traditional method and the LOI technique demonstrating that the LOI
method was reliable and could provide accurate estimates of SOC and SIC for
arid soils. In the same year Ghimire et al analysed 200 soil samples from 5
different soil depths of Rampur and Bareini across Chitwan valley to evaluate
precision of loss on ignition method of SOC analysis. The SOC values
obtained were compared with soil organic carbon values from dry combustion
method of SOC analysis for some soil samples in which the correlation and
regression analysis showed precise results of SOC from both locations.
Tuffour et al (2014) worked on the estimation of soil organic carbon by
relating Walkley Black and Wet oxidation method to the loss on ignition for 12
soil samples from 0-15 cm depth collected from 4 sites of the crop plantation
section of the Department of Crop and Soil Sciences, KNUST. The results
showed that the highest estimate of SOC 3.28% was produced by LOI method
whereas WB gave lower estimates with 1.35% being highest produced by this
method. Very weak relationship was observed between LOI and WB
calculations. Comparison of different methods for the determination of total
organic carbon and humic substances in Brazilian soils was done by
Fernandes et al (2014) in 17 Brazilian soil samples of different classes and
textures by dichromate oxidation method and loss-on-ignition method at 450°C
during 5 h and at 600°C during 6 h and by dry combustion method. The
amount of Organic Carbon was overestimated by Loss-on-ignition method
while the WalkleyBlack method underestimated the OC contents of humic
fractions, which was associated with the partial oxidation of the humin
fraction. Bojko and Kabala (2014) also conducted a study for the estimation
of total organic carbon in the mountain soils of the Karkonosze Mountain by
collecting 476 mineral and 79 organic samples from 31 soil profiles located in
different altitude zones. LOI determined by drying-weighing and TOC by the
dry combustion method with CO2 absorption showed that the average of the
LOI/TOC ratio was about 2, but varied with LOI value.
Hoogsteen et al (2015) carried out many experiments to estimate soil organic
carbon through loss on ignition method and found that a large number of
factors such as furnace type, sample mass, duration and temperature of ignition
and clay content of samples influence its accuracy. The LOI increased with
duration at lower temperatures (550°C) for sandy soil while at greater
temperatures (600°C and 650°C) no effect of duration was found. The SOM to
SOC conversion factor decreased at an ignition duration of 3 h from 0.70
(350°C) to 0.57 (500°C) and stabilized around 0.55 between 550°C and 650°C
indicating that at temperature ≥ 550°C all SOM had been removed. In the same
year Wood worked on the determination of moisture content and total organic
carbon within Basin Environments by Loss-on-ignition by adopting two phases
samples which were initially dried and were then ignited at elevated
temperatures to burn off all organic carbon, thus providing a measure of
moisture and organic content respectively.
El-Hussieny (2017) compared three methods including relatively high-
temperature Loss-onignition (LOI) 550°C , relatively Low-temperature LOI
(375°C) and wet digestion with chromic acid in Walkley-Black method for
organic carbon estimation to develop a correlation model between the standard
method and the other applied techniques to further tuning of previously
estimated ecosystems under similar conditions. The results showed that
precautions are needed while using the high-temperature LOI in order to
minimize the overestimation of SOC due to loss of inorganic fraction on high
temperatures. Further the low-temperature LOI approach could be considered
as an accurate, simple, fast, cost effective and eco-friendly method for
estimation of SOC.
Paramanthan et al (2018) conducted a study to investigate the applicability of
common and routine conversion factor to determine SOM from OC of tropical
peats. Samples from six peat profiles all >150 cm or deep, from a peat forest
reserve and an oil palm plantation in Malaysia were analysed. A comparison of
C-values derived from CNS, WB and LOI methods indicated that the use of
LOI for tropical organic soils provide a better estimation of organic matter
(including organic carbon) than the Walkley Black carbon or CNS data. It also
provides a simple measure for peat classification when using conversion
factors to determine SOM. It is also proposed that the LOI rather than WB-C
or CNS methods may be used to define organic soil materials and Histosols for
tropical lowland organic soils.
Kumar et al (2019) attempted to investigate C-equivalent correction factor for
SOC by WalkleyBlack (wet oxidation) and loss-on-ignition LOI methods in
relation to TOC analyzer (dry combustion) method which TOC analyser
method to be the best method of total soil organic carbon estimation. C-
equivalent correction factor ranged from 1.10 to 1.17 for SOC determination
by WalkleyBlack method to TOC analyzer method, whereas it varied from
0.257 to 0.417 for soil organic matter (SOM) by LOI method to TOC analyzer
for soils under various land use/ land cover types in the Himalayan region.

STUDY AREA

The present study entitled “Estimate Soil Organic Carbon in soils of Kashmir
using Loss on ignition” was carried out on soils of Kashmir collected from
different districts of Kashmir valley. The details of the study site and other
features of the study area were described below:
Study site
The study was conducted on soil samples collected from different districts of
North, Central and South Kashmir. The geographical location and
physiographic features of study area are given below.
Geographical location
The Kashmir Valley, also known as the Vale of Kashmir, is an intermontane
valley in the northern Himalayas. The valley is bounded on the southwest by
the Pir Panjal Range and on the northeast by the main Himalayas range. It is
approximately 135 km long and 32 km wide, and drained by the Jhelum River.
It is divided into three regions North, Central and South Kashmir.
Shopian is a hill district with its administrative division in Shopian, located in
the Indian union territory of Jammu and Kashmir having coordinates: 33.72°N
74.83°E, since it is situated on the historical road commonly known as Mughal
Road, most of its area is occupied by forests. Shopian district comes under the
Pir Panjal Range which makes it very cold in winter.
Kulgam is a town having coordinates: 33°38′24″N 75°01′12″E is located at a
distance of 67 km from the summer state capital of Srinagar. Pulwama district
with geo-coordinates: 33.88°N 74.92°E and is almost 25 km from the summer
capital of Srinagar. It is often called the "Anand of Kashmir" (the joy, the
delight), and the "Dudha-Kul of Kashmir" (the milk) on account of its high
milk production.
Karnah is an administrative tehsil of the Kupwara district in Jammu and
Kashmir. It has 42 villages out of which 40 have population and is 78 km away
from the main town of Kupwara. Uri is a town and a tehsil in the Baramulla
district with geo- coordinates: 34°5′10″N 74°2′0″E. It is located on the left
bank of the Jhelum River, about 10 km east of the Line of Control with
Pakistan.
Bandipore district is one of the 22 districts in Jammu and Kashmir with geo-
coordinates of 34°25′12″N 74°39′00″E is a township with peculiar scenic
beauty and is located in the foothills of the snowclad peaks of Harmukh
overlooking the shores of Wular. The district is bounded by Kupwara district
in the west, Baramulla district in the south and Kargil, Srinagar and Ganderbal
districts in the east.
Ganderbal district, with geo-coordinates of 33.73°N 75.15°E located at an
average elevation of 1,950 m above sea level, at a distance of 21 km from
Srinagar city spread across the Sind River. Tangmarg is famous for fresh cold
water, heavy snowfall, and tourism. It is a hilly area with most parts covered
by lush green forests within geo-coordinates of 34°03′33″N 74°25′28″E,
Tangmarg is 39 km (24 mi) from Srinagar and has many tourist spots like
Drung, Gulmarg, Baderkoot, Zandpal, Gogaldara, Nigli Nullah and Baba
Reshi. Srinagar is the largest city and the summer capital of this valley which
lies within geo-coordinates of 34°5′24″N 74°47′24″E on the banks of the
Jhelum River, a tributary of the Indus, and Dal and Anchar lakes. The city is
known for its natural environment, gardens, waterfronts and houseboats.
Fig. 1. Map showing outline of the Kashmir valley border
Fig. 2. Map showing different districts of the Kashmir valley

Topography and Soil

The topography of the state is such that low-lying valleys are surrounded by
high mountain ranges of the Himalayas. Of all the valleys, the most important
one, the Kashmir valley lies between the coordinates 33º 20' to 34º 54' North
latitude and 73º 55’ to 75º 35' East longitude. It is situated in the lap of the
Western Himalayas and decorated by snow-covered, silver headed mountains,
magical lakes, green grasslands and has enjoyed the reputation of being home
of herbal medicines. The valley is located on an average height of 1,700m
above the sea level and is encompassed by mighty Himalayan ranges
occupying an area of 15,948 sq. km. with forest area about 8,123 sq. km.
The Kashmir valley lies in the temperate zone with an alluvial soil rich in
nitrogen and organic matter. There are different types of soils in the valley
which include slit (Gurti), loam (Bahil), sandy (Sekil), vegetable soil
(Surzamin), kerewa soil (Wuder) and peaty (Nambal soil).

Climate
Kashmir valley has a moderate climate, which is largely defined by its
geographic location, with the towering Karakoram Range in the north, Pir
Panjal Range in the south and west and Zanskar Range in the east. It can be
generally described as cool in the spring and autumn, mild in the summer and
cold in the winter. As a large valley with significant differences in
geolocations among various districts, the weather is often cooler in the hilly
areas compared to the flat lower part.
Summer is usually mild and fairly dry, but relative humidity is generally high
and the nights are cool. The precipitation occurs throughout the year and no
month is particularly dry. The hottest month is July and the coldest are
December-January.
Kashmir valley enjoys a more moderate climate but weather conditions are
unpredictable. The recorded high temperature is 33 oC and the recorded low is -
18oC. Altitude determines the degree of coolness, precipitation and summer
temperature. The sub-Mediterranean climate of valley receives an average
rainfall of about 65cm. Jhelum is the only river bypassing through the
Himalayan lap in Kashmir valley. In the valley of Kashmir, winter is chilling
cold and lasts from December to March with minimum temperature falling
down up to -2ºC and maximum rises up to 14ºC. There are strong winds,
snowfall and rainfall during this period. Warmer weather starts in April and
lasts till November with maximum temperature of 36ºC and minimum of 14ºC.
Methodology
Soil organic carbon (SOC) is the carbon that remains in the soil after partial
decomposition of any material produced by living organisms. It constitutes a
key element of the global carbon cycle through atmosphere, vegetation, soil,
rivers and the ocean. SOC is the main component of soil organic matter (SOM)
and is the critical component of soil resource base. The role of soil organic
carbon in formation of stable soil aggregates has major implications on air
water balance and surface strength of soil (Scholes et al., 1994). Moreover, the
soil carbon pool and soil processes are the important regulators of CO 2 in
atmosphere (Lal et al., 1999). Beneficial effects in crop production include
SOC acting as a source of major plant nutrients, a promoter of favourable soil
conditions, soil biota population and nutrient cycling processes (Goh, 2004;
Ghimire et al., 2013). Soil organic carbon has to be periodically measured not
only for study of climate change but also for study of ecology.
Loss-on-ignition has been considered as a rapid, inexpensive and convenient
method for estimating soil organic carbon, which involves dry combusting the
samples at high temperatures in a muffle furnace (Rahman et al., 2011). It is
relatively quick and inexpensive method for determining the organic carbon
throughout core lengths (Heiri et al., 2001). The technique has been used to
assess forest surface soils (De Vos et al., 2005), to identify sedimentological
changes associated with tsunami phases (Hawkes et al., 2007) and has also
been adopted in many other environmental settings (Wood, 2015). Loss-on-
ignition is one of the most widely used methods for measuring organic matter
and carbon 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 (Hoogsteen
et al., 2015).
Sample collection
Soil samples comprising of agricultural, forest and lawn soils were collected
from two depths (0-10 cm and 10-20 cm) and in separate polythene bags from
different regions of Kashmir valley. Then, these samples were air dried,
grinded and passed through a 2mm sieve for further processing. (Wright et al.,
2007)
Loss-on-ignition
The loss-on-ignition procedure prescribed by Hoogsteen et al. (2015) was used
for analysing the organic carbon content in soil samples collected from
different regions of Kashmir valley. A 20-gram sample was placed in crucibles
that were pre-weighed and pre-heated at 105°C, then cooled.
Crucibles with soil samples were then handled as per following procedure:
1. Heated in a in drying oven at the initial (preparation) temperature
overnight.
2. Cooled to room temperature in a desiccator.
3. Weighed the crucibles + sample and reweigh at 105°C.
4. Placed into muffle furnace and heated at the ignition temperature of
550°C for 3h.
5. Removed from furnace and cool to room temperature in a desiccator.
6. Weighed the ignited samples and recorded the weight.

The mass of soil loss was expressed on a dry weight basis by the following
equation:
LOI (g kg-1) = (Weight initial T – Weight ignition T) / Weight initial T × 1000
The loss in weight of soil was taken as a raw measure of organic carbon
content (Konare et al., 2010).
Results and Discussion

With the objective of Estimating the organic carbon content in the soils of
Kashmir valley, a number of soil samples were taken from agricultural, forest
and garden soils from different districts of Kashmir valley at two depths (0-10
cm and 10-20 cm). In total, 42 soil samples, including 14 agricultural soil
samples, 14 Forest soil samples, 14 Garden/Lawn soil samples. After
collecting the soil samples in zipper bags the samples were taken to lab for
analysis of soil organic carbon using Loss on Ignition method by heating the
samples at a temperature of 550oC for 3 hours in the muffle furnace. The
overall scenario of organic carbon showed a good amount in the samples taken
from agricultural soil of Karnah, forest soil of Shopian, Ganderbal, and garden
soil of Ganderbal while as lower amount of organic carbon was found in the
samples taken from garden soil of Tangmarg and Agricultural land soil of
Kulgam and Bandipora. A high mean value of LOI (g C kg -1) in samples of
Forest soil, Agricultural soil taken at 0-10 cm depth and 10-20 cm depth
respectively and mean value of LOI (g C kg-1) in samples of Garden/ Lawn
soils was found low at both the depths.

The soil samples analysed for estimation of soil organic carbon by loss on
ignition method taken as a raw measure of organic carbon content produced
the following findings:

• The amount of organic carbon was found to be more in the upper layers
(0-10 cm depth) in Garden/ Lawn and Forest soils while the amount of
organic carbon was found to be more in lower layers (10-20 cm depth)
in the Agricultural soils.
• The amount of organic carbon varied greatly from land to land
depending upon their usage and environment. It also varied with soil
 depth, soil type and terrain of the area from which the samples were
taken.

Agricultural soils

The estimation of organic carbon in soil samples collected from agricultural

areas using loss on ignition technique showed a good amount of soil organic
carbon in soil samples taken at a depth of 0-10 cm from Karnah, Uri and
Shopian district of Kashmir and a less amount of organic carbon was found in
the said samples taken from a depth of 10-20 cm. However, the soil samples
collected at a depth of 0-10 cm from Kulgam, Khajopora, Pulwama and
Bandipora district of Kashmir showed an opposite trend. The decrease in the
soil organic carbon levels in these soil samples may be due to the reason that
these samples were taken from orchards as there is a lesser organic matter
accumulation and excessive use of fertilizers in these fields lead to lower level
of soil organic carbon content in such soil. The less organic carbon content in
Bandipora could be due to its sloppy terrain where the rain water runoff take
away all the materials from the soil surface leading to lesser organic carbon
content in the upper layer. The results are in consonance with the studies of Six
et al., 1998, Balesdent et al., 2000 and Anderson., 2005, which observed that
loss of soil organic carbon in cultivated soils can be attributed to erosion, lower
C inputs in croplands, a reduced stabilization of SOM due to deteriorated
aggregation, and a subsequent mineralization promoted by increased soil
temperature and aeration. The overall observation of results (Fig. 1) of soil
organic matter in the agricultural soils indicates that the organic matter content
was highest in Karnah followed by Uri, Shopian, Pulwama, Khajopora and
Kulgam.
 Agricultural/Orchard land soil LOI g C kg -1
120
100

80
60

40
20

0
Shopian Kulgam Khajopora Pulwama Karnah Uri Bandipora
0-10 cm 10-20 cm

Fig 1. Soil organic carbon in Agricultural soils taken from different areas of
Kashmir valley.

Forest soils

The analysis of samples taken from different forest using loss on ignition
technique for estimation of organic carbon at two depths (0-10 cm and 10-20
cm) showed that a high amount of organic carbon was present in the soil
samples taken at 0-10 cm depth. While as the second set of samples taken at a
depth of 10-20 cm showed a lower amount of organic carbon (Fig. 2). This
could be attributed to the accumulation of fresh and decomposed organic
matter in the form of leaf litter and other plant products on the upper layer of
the forest soils as a study on soil organic carbon content in forests showed that
are under temperate climatic conditions, soil organic carbon stocks under
coniferous species are higher in the upper layers, particularly due to an
accumulation of acidic litter. (Jandl et al., 2007; Oostra et al., 2006; Schulp et
al., 2008). Another study conducted by Kafle (2019) showed a similar trend as
soil organic carbon was found decreasing with increased soil depths, with a
statistically significant difference in values across different soil layers. Organic
carbon was found higher at the upper level of soil in almost all cases. It was
further observed that the greater the depth, the lower the organic carbon
content in the forest soils. (Pradhan et al., 2012). Overall observation of the
results of LOI soil organic carbon in the seven-forest soil type of different
areas showed that the higher organic carbon content was present in forest soil
of Shopian followed by Ganderbal, Uri, Burzahama, Bandipora, Karnah, and
Kulgam.

Forest soil LOI g C kg -1

100
90
80
70
60
50
40
30
20
10
0
Shopian Bandipora Karnah Uri Ganderbal Kulgam Burzahama
0-10 cm 10-20 cm

Fig 2. Soil organic carbon in Forest soils taken from different areas of
Kashmir valley.
Garden/Lawn soils
The data in fig 3 shows the amount of soil organic carbon present in the soil
samples taken from Gardens/Lawns of different houses at two depths (0-10 cm
and 10-20 cm). The analysis of soil organic carbon in the soil samples showed
that there was a higher amount of organic carbon present in the upper layer (0-
10 cm) and a lesser amount is present in lower layers (1020 cm) of most of the
samples with exception of soil samples collected from the Sanatnagar area of
Srinagar and Budgam district. In these samples the amount of organic carbon
in the upper layer was lesser and the amount of organic carbon in lower layers
was higher. The overall organic carbon content in the garden soils was higher
in Garden soils was higher in Ganderbal followed by Shopian, Karnah and
Tangmarg, our results were in consonance with the results of Edmond et al.,
(2014) who observed that lowering down of organic carbon with increasing
depths in domestic gardens.

Lawn/Garden soil LOI g C kg -1

100
90
80
70
60
50
40
30
20
10
0
Shopian Ganderbal Sanatnagar Budgam Bandipora Tangmarg Karnah
0-10 cm 10-20 cm

Fig 3. Soil organic carbon in Lawn/Garden soils taken from different areas of
Kashmir valley.
This is a likely consequence of garden management practices that include
additions of organic matter such as peat, composts organic fertilisers and
mulches, and the contribution of woody trees and shrubs that tend to enhance
SOC stocks (Bradley et al.,2005; Osmond and Hardy, 2004; Robbins and
Birkinholtz, 2003) as seen in our study.
Mean value of soil organic Mean value of soil organic
carbon g C kg-1 carbon g C kg-1
70 75

65 70

60 65

55 60

50 55
Agricultural Lawn/Garden Forest Forest Agricultural Lawn/Garden

10-20 cm 0-10 cm

Fig. 4 Mean value of SOC g C kg-1 in Forest, Agricultural and Lawn soils
The mean value of soil organic carbon calculated from the data found by
analysing all three sets of samples from Agricultural, Forest and Garden/Lawn
soils indicated that the forest soils had a mean soil organic carbon of 73.10 g C
kg-1, 56.20 g C kg-1 in first and second soil layer respectively. The agriculture
soils had a mean soil organic carbon of 63.17 g C kg-1, 67.28 g C kg-1 in first
and second soil layer soil layer respectively and the garden/lawn soils had a
mean soil organic carbon of 62.25 g C kg-1 and 57.55 g C kg-1 in the two soil
depths respectively (Fig. 4). Based on the results it was found that forest soil
samples had higher mean organic carbon than agricultural and garden soils
taken at 0-10 cm depth and the mean soil organic carbon in the samples taken
at 10-20 cm depth was found to be higher in agricultural soils as compared to
the forest and garden/Lawn soils. This could be due to the maximum litter fall
and plant residues associated with microbial activities observed in the forests,
which shows the interlinkage of forest ecosystems in storage or sequestration
of SOC pools compared to other lands and the same reason was cited by (Iqbal
and Tiwari, 2016) in their study. Soil Organic Carbon was found decreasing
with increased soil depths, with a
statistically significant difference in values among across different soil layers.
The topsoil containing higher amounts of SOC, are attributed to the forest
management practices retaining organic matter in the forest floor (Kafle.,
2019). The reason for increase in the mean soil organic carbon in agricultural
land maybe due to mixing up of extra organic matter in fields in the form of
cow dung, crop residues besides the use of biofertilizers in the field to increase
the yield.
 Organic carbon percentage 0-10 cm

31% 32%
Agricultural
Forest
Lawn/Garden

37%

Fig 5. Percentage of organic carbon content Agricultural, Forest and Lawn

soils (0-10 cm).
The data in Fig 5 shows percentage of organic carbon upto a depth of 0-10 cm
in Agricultural, Garden and Forest soils. Analysis of the results show that the
organic carbon percentage was more in forest soils (37%) followed by
Agricultural soils (32%) and garden/lawn soils (31%).

Organic carbon percentage 10-20 cm

31%
36% Agricultural
Forest
Lawn

33%

Fig 6. Percentage of organic carbon content in Agricultural, Forest and Lawn

soils.
However, the percentage of organic carbon content in the soil samples taken at
(10-20 cm depth
(Fig. 6) was found to be more in agricultural soils (37%) organic carbon
followed by Garden/Lawn soils with (32%) organic carbon and forest soils
with (31%).

32% 32%
Forest
Agricultural
Garden/Lawn

36%

Fig 7. Percentage share of Soil organic carbon between Agricultural, Forest

and Garden/Lawn soils.

Percentage share of soil organic carbon in soils of Forest land, Agricultural

land and
Garden/lawns soils calculated from the obtained data (Fig. 7) showed that the
forest soils had 36% of the total soil organic carbon followed by agricultural
soils and garden/lawn soil with 33% and 31% respectively. The organic carbon
pool under forest land use was higher compared to the other land uses. This
could be due to the maximum litter fall and plant residues associated with
microbial activities observed in the forests, which show the interlinkage of
forest ecosystems in storage or sequestration of soil organic carbon pools
compared to other land uses Sharma et al., (2013), Iqbal and Tiwari, (2016)
carried out some studies on soil organic carbon pool and their result were
similar to those of ours.
Conclusion:

Soil organic carbon is a key element of the global carbon cycle. It is the main
component of soil organic matter and is the critical component of soil resource
base. Thus, SOC has to be periodically measured not only for study of climate
change but also for study of ecology. In this backdrop the soil organic carbon
estimation in Kashmir soils using LOI (loss on ignition) method produced the
following findings:
• The amount of carbon was found to be more in upper layers (0-10 cm)
than in lower layers (10-20cm).
• The amount of carbon varied from land to land depending upon usage
and environment of the area.
• The amount of soil organic carbon depends on many factors such as type
of soil, depth of soil and terrain of area.
 • Soil organic carbon is present in large quantities in the agricultural soils
due to addition of organic like cow dung and crop residues etc. in the
fields.
• The organic carbon content present in forest soils is mainly due to native
organic matter which gets accumulated in the form of leaf litter and
plant residues of plant present in the forest soils.
• The forest soils highly contribute to the organic carbon content as
compared to the agricultural and garden soils.

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