Loss on ignition (LOI) is a test used in inorganic analytical chemistry and soil science, particularly in the analysis of minerals and the chemical makeup of soil. It consists of strongly heating ("igniting") a sample of the material at a specified temperature, allowing volatile substances to escape, until its mass ceases to change. This may be done in air or in some other reactive or inert atmosphere. The simple test typically consists of placing a few grams of the material in a tared, pre-ignited crucible and determining its mass, placing it in a temperature-controlled furnace for a set time, cooling it in a controlled (e.g., water-free, CO2-free) atmosphere, and re-determining the mass. The process may be repeated to show that the mass change is complete. A variant of the test in which mass change is continually monitored as the temperature changes is called thermogravimetry.
The loss on ignition is reported as part of an elemental or oxide analysis of a mineral. The volatile materials lost usually consist of 'combined water' (hydrates and labile hydroxy-compounds) and carbon dioxide from carbonates. It may be used as a quality test, commonly carried out for minerals such as iron ore. For example, the loss on ignition of fly ash is composed of contaminants and unburnt fuel.
In pyroprocessing industries such as lime,calcined bauxite, refractories or cement manufacture, the loss on ignition of the raw material is roughly equivalent to the mass loss it will experience in a kiln. Likewise, in minerals, the loss on ignition indicates the material actually lost during smelting or refining in a furnace or smelter. The loss on ignition of the product indicates the extent to which the pyroprocessing was incomplete. ASTM tests are defined for limestone and lime [1] and cement [2] among others.
Soil is composed of living organisms, water, carbonates, carbon containing material, decomposing matter and much more. To determine how much one of these soil components make up the entire soil mass, the LOI procedure is implemented. Initially, the researcher will take the mass of the sample prior to LOI and then place the sample into a heating device. Depending on what the researcher is trying to determine in the soil, the temperature of the device can be set to the corresponding temperature. The soil sample is kept at this temperature for an extended period of time after which it is removed and allowed to cool down before re-weighing the sample. The amount of mass lost after the LOI treatment is equal to the mass of the component the researcher is trying to determine. The typical set of materials needed to use LOI include: a high precision mass balance, a drying oven, temperature controlled furnace, preheated crucibles and soil sample from the location of interest.
There are many ways to properly utilize loss on ignition for scientific research. [3] A soil sample left overnight in a drying oven at 100 °C would have its water content completely evaporated by morning. [4] This could allow the researchers to determine the amount of water initially in the soil sample and its porosity by comparing the change in weight of the sample before and after the evaporation. This new weight of the sample is called the dry weight and its previous weight is called the wet weight.
A general procedure of how to perform a loss on ignition is as follows: [5]
Typically, this method is used to determine water content levels, carbon levels, amount of organic matter levels, amount of volatile compounds. [6] LOI is also used in the cement industry which operates the furnace in the 950 °C range (e.g. cement kilns), combustion engineers also use LOI but at temperatures lower than 950 °C range. [7]
In many research labs, the use of asbestos gloves is required when operating the furnace because it can reach very high temperatures. [6] The use of face masks is also recommended at higher temperatures to ensure the safety of researchers and junior lab members. [8] It is also recommended that researchers performing the LOI procedure remove all jewelry and watches as they are excellent conductors of heat. When removing samples at high temperatures, these accessories can easily heat up and result in burns. [9]
The cement industry uses the LOI method by heating a cement sample to 900-1000 °C until the mass of the sample stabilizes. Once the mass stabilizes, the mass loss due to LOI is determined. This is usually done to assess the high water content in the cement or carbonation, as these factors diminish the quality of cement. [10] High losses are generally attributed to poor cement storage conditions or manipulation of cement quality by suppliers. This practice ensures that the cement used on a site adheres to the correct composition, meeting safety protocols and customer requirements.
In the mining industry, the utilization of LOI is essential for determining the moisture and volatile material present in the rock. Thus, when performing whole-rock analysis to ascertain total volatiles, the LOI method is employed. To eliminate all volatiles and convert all iron into iron oxides, the LOI temperature is set at 900-1000 °C.
Portland cement is the most common type of cement in general use around the world as a basic ingredient of concrete, mortar, stucco, and non-specialty grout. It was developed from other types of hydraulic lime in England in the early 19th century by Joseph Aspdin, and is usually made from limestone. It is a fine powder, produced by heating limestone and clay minerals in a kiln to form clinker, grinding the clinker, and adding 2 to 3 percent of gypsum. Several types of portland cement are available. The most common, called ordinary portland cement (OPC), is grey, but white portland cement is also available. Its name is derived from its resemblance to portland stone which was quarried on the Isle of Portland in Dorset, England. It was named by Joseph Aspdin who obtained a patent for it in 1824. His son William Aspdin is regarded as the inventor of "modern" portland cement due to his developments in the 1840s.
Differential scanning calorimetry (DSC) is a thermoanalytical technique in which the difference in the amount of heat required to increase the temperature of a sample and reference is measured as a function of temperature. Both the sample and reference are maintained at nearly the same temperature throughout the experiment. Generally, the temperature program for a DSC analysis is designed such that the sample holder temperature increases linearly as a function of time. The reference sample should have a well-defined heat capacity over the range of temperatures to be scanned. Additionally, the reference sample must be stable, of high purity, and must not experience much change across the temperature scan. Typically, reference standards have been metals such as indium, tin, bismuth, and lead, but other standards such as polyethylene and fatty acids have been proposed to study polymers and organic compounds, respectively.
A crucible is a ceramic or metal container in which metals or other substances may be melted or subjected to very high temperatures. Although crucibles have historically tended to be made out of clay, they can be made from any material that withstands temperatures high enough to melt or otherwise alter its contents.
The flash point of a material is the "lowest liquid temperature at which, under certain standardized conditions, a liquid gives off vapours in a quantity such as to be capable of forming an ignitable vapour/air mixture".
The autoignition temperature or self-ignition temperature, often called spontaneous ignition temperature or minimum ignition temperature and formerly also known as kindling point, of a substance is the lowest temperature in which it spontaneously ignites in a normal atmosphere without an external source of ignition, such as a flame or spark. This temperature is required to supply the activation energy needed for combustion. The temperature at which a chemical ignites decreases as the pressure is increased.
The cone penetration or cone penetrometer test (CPT) is a method used to determine the geotechnical engineering properties of soils and delineating soil stratigraphy. It was initially developed in the 1950s at the Dutch Laboratory for Soil Mechanics in Delft to investigate soft soils. Based on this history it has also been called the "Dutch cone test". Today, the CPT is one of the most used and accepted soil methods for soil investigation worldwide.
Gravimetric analysis describes a set of methods used in analytical chemistry for the quantitative determination of an analyte based on its mass. The principle of this type of analysis is that once an ion's mass has been determined as a unique compound, that known measurement can then be used to determine the same analyte's mass in a mixture, as long as the relative quantities of the other constituents are known.
Soil mechanics is a branch of soil physics and applied mechanics that describes the behavior of soils. It differs from fluid mechanics and solid mechanics in the sense that soils consist of a heterogeneous mixture of fluids and particles but soil may also contain organic solids and other matter. Along with rock mechanics, soil mechanics provides the theoretical basis for analysis in geotechnical engineering, a subdiscipline of civil engineering, and engineering geology, a subdiscipline of geology. Soil mechanics is used to analyze the deformations of and flow of fluids within natural and man-made structures that are supported on or made of soil, or structures that are buried in soils. Example applications are building and bridge foundations, retaining walls, dams, and buried pipeline systems. Principles of soil mechanics are also used in related disciplines such as geophysical engineering, coastal engineering, agricultural engineering, hydrology and soil physics.
Thermogravimetric analysis or thermal gravimetric analysis (TGA) is a method of thermal analysis in which the mass of a sample is measured over time as the temperature changes. This measurement provides information about physical phenomena, such as phase transitions, absorption, adsorption and desorption; as well as chemical phenomena including chemisorptions, thermal decomposition, and solid-gas reactions.
Elemental analysis is a process where a sample of some material is analyzed for its elemental and sometimes isotopic composition. Elemental analysis can be qualitative, and it can be quantitative. Elemental analysis falls within the ambit of analytical chemistry, the instruments involved in deciphering the chemical nature of our world.
Water content or moisture content is the quantity of water contained in a material, such as soil, rock, ceramics, crops, or wood. Water content is used in a wide range of scientific and technical areas, and is expressed as a ratio, which can range from 0 to the value of the materials' porosity at saturation. It can be given on a volumetric or mass (gravimetric) basis.
In analytical chemistry, ashing or ash content determination is the process of mineralization for preconcentration of trace substances prior to a chemical analysis, such as chromatography, or optical analysis, such as spectroscopy.
Coal analysis techniques are specific analytical methods designed to measure the particular physical and chemical properties of coals. These methods are used primarily to determine the suitability of coal for coking, power generation or for iron ore smelting in the manufacture of steel.
Geotechnical investigations are performed by geotechnical engineers or engineering geologists to obtain information on the physical properties of soil earthworks and foundations for proposed structures and for repair of distress to earthworks and structures caused by subsurface conditions; this type of investigation is called a site investigation. Geotechnical investigations are also used to measure the thermal resistance of soils or backfill materials required for underground transmission lines, oil and gas pipelines, radioactive waste disposal, and solar thermal storage facilities. A geotechnical investigation will include surface exploration and subsurface exploration of a site. Sometimes, geophysical methods are used to obtain data about sites. Subsurface exploration usually involves soil sampling and laboratory tests of the soil samples retrieved.
A sieve analysis is a practice or procedure used in civil engineering and chemical engineering to assess the particle size distribution of a granular material by allowing the material to pass through a series of sieves of progressively smaller mesh size and weighing the amount of material that is stopped by each sieve as a fraction of the whole mass.
The Proctor compaction test is a laboratory method of experimentally determining the optimal moisture content at which a given soil type will become most dense and achieve its maximum dry density. The test is named in honor of Ralph Roscoe Proctor, who in 1933 showed that the dry density of a soil for a given compactive effort depends on the amount of water the soil contains during soil compaction. His original test is most commonly referred to as the standard Proctor compaction test; his test was later updated to create the modified Proctor compaction test.
A metallurgical assay is a compositional analysis of an ore, metal, or alloy, usually performed in order to test for purity or quality.
Headspace gas chromatography uses headspace gas—from the top or "head" of a sealed container containing a liquid or solid brought to equilibrium—injected directly onto a gas chromatographic column for separation and analysis. In this process, only the most volatile substances make it to the column. The technique is commonly applied to the analysis of polymers, food and beverages, blood alcohol levels, environmental variables, cosmetics, and pharmaceutical ingredients.
The term "lignin characterization" refers to a group of activities within lignin research aiming at describing the characteristics of a lignin by determination of its most important properties. Most often, this term is used to describe the characterization of technical lignins by means of chemical or thermo-chemical analysis. Technical lignins are lignins isolated from various biomasses during various kinds of technical processes such as wood pulping. The most common technical lignins include lignosulphonates, kraft lignins, organosolv lignins, soda lignins and lignin residue after enzymatic treatment of biomass.