ISO/TC 27/SC 5 - Methods of analysis

This document defines terms that are used in connection with both maceral and microlithotype analyses, and with the determination of the reflectance of vitrinite. It applies to the terms used in the examination of coal of all ranks and types. This document is not intended to be a comprehensive glossary of coal petrographic terminology, nor does it attempt to provide sufficient information to allow recognition of all the coal components described.

This document specifies methods for preparing a polished particulate block from a sample of crushed coal for analysis by reflected light microscopy. These methods can also be applied to the preparation of a polished, embedded lump of coal.

This document specifies a method for determining the proportions of the maceral groups (and the minerals, if desired) in coals. It is concerned only with determinations made on polished particulate blocks using incident white light. For lower-rank coals, the additional use of the fluorescence mode is necessary to identify liptinites.

This document specifies a method, using a graticule with 20 crossline intersections, for determining the proportions of microlithotypes, carbominerite and minerite in coals. It applies only to determinations made on polished particulate blocks using reflected white light. Additional blue, blue-violet or UV light excitation for better identification of liptinite in fluorescence can be used especially for low rank coals.

This document specifies the methods for determining the reflectance of vitrinite of coals microscopically on polished surfaces, immersed in oil. The methods are applicable to coals from single seams or coal blends covering the whole range of low-, medium- and high-rank coal. Vitrinite reflectance measurements can be used to characterize the components within blends. Measures can be taken to correct for the vitrinite percentage within each of the components of the blend or to determine the proportion of components in a blend, particularly when the components have dissimilar vitrinite contents. This method necessitates the identification of vitrinite by the analyst. Reflectance measurements on vitrinite, obtained by interpreting the results from an automated system, are outside the scope of this document.

This document establishes a classification of brown coals and lignites by types on the basis of total moisture mass fraction and tar yield.

This document describes a method for the measurement of the swelling properties of hard coal using a dilatometer.

This document specifies a method for the determination of the gross calorific value of coal and coke at constant volume and at the reference temperature of 25 °C in a combustion vessel calorimeter calibrated by combustion of certified benzoic acid. The result obtained is the gross calorific value of the analysis sample at constant volume with all the water of the combustion products as liquid water. In practice, fuel is burned at constant (atmospheric) pressure and the water is not condensed but is removed as vapour with the flue gases. Under these conditions, the operative heat of combustion is the net calorific value of the fuel at constant pressure. The net calorific value at constant volume can also be used; formulae are given for calculating both values. General principles and procedures for the calibrations and the fuel tests are specified in the main text, whereas those pertaining to the use of a particular type of calorimetric instrument are described in Annexes A to C. Annex D contains checklists for performing calibration and fuel tests using specified types of calorimeters. Annex E gives examples illustrating some of the calculations. Annex F provides guidance around safe use, maintenance and testing of the calorimeter combustion vessel. NOTE Descriptors: solid fuels, coal, coke, tests, determination, calorific value, rules of calculation, calorimetry.

This document specifies a method of determining the amount of mineral matter in all types of coal, including brown coals and lignites.

This document specifies a method of determining the total carbon and the total hydrogen in coal and coke, by the Liebig method.

This document specifies a method of determining the characteristic fusion temperatures of ash from hard coal. NOTE Descriptors: fossil fuels, ash, ashes, tests, high temperature tests, determination, and fusibility.

This document describes the extraction from coal by dilute hydrochloric acid and determination of extractable sodium, potassium, calcium, iron and magnesium.

This document specifies a procedure for the determination of the total cadmium mass fraction of coal.

This document specifies a reduced molybdophosphate photometric method for the determination of the total phosphorus mass fraction of hard coal, lignites and coke. Two methods for taking the phosphorus into solution are specified, namely extraction from the coal or coke ash with acid or by repeated oxidation of the coal or coke, by acid, to remove carbonaceous matter.

This document specifies a method using Eschka's mixture during ashing, extraction of the ash residue with acid, and hydride generation atomic absorption spectrometry or hydride generation atomic fluorescence spectrometry, for the determination of arsenic and selenium in solid mineral fuels. The method is also applicable for the determination of the analytes by hydride generation inductively coupled plasma atomic emission spectrometry.

This document specifies a method of determining the mass fraction of acetone-soluble material (“resinous substance”) in the benzene-soluble extract from brown coals and lignites. NOTE The acetone extract also contains a mass fraction of wax dissolved simultaneously with the "resinous substance".

This document specifies a method of determining the total carbon and the total hydrogen in coal and coke by a high temperature combustion method.

This document specifies a method for obtaining a relative measure of the plastic behaviour of hard coal when heated under prescribed conditions. The method is used to obtain values of the plastic properties of coals and blends used in carbonization and in other situations where determination of plastic behaviour of coals is of practical importance. NOTE The empirical nature of this test requires proper equipment calibration to produce fluidity readings which are a true indication of the relative plastic behaviour of the coal.

This document specifies methods of determining the sulfate and pyritic sulfur mass fraction of coals, and of calculating the amount of organic sulfur present.

This document specifies the Gray-King coke method of assessing the caking power of hard coal under standard conditions.

This document specifies a procedure for the determination of the total mercury mass fraction of coal.

This document specifies a method for the determination of the moisture in the analysis sample of brown coals and lignites using an indirect gravimetric method.

This document specifies two methods for determination of the total moisture of brown coals and lignites using an indirect gravimetric single-stage method and a two-stage method.

This document specifies a method for determining the swelling properties of hard coal when heated in a covered crucible. NOTE The "crucible swelling number" (CSN) is also known as the "free swelling index" (FSI).

This document specifies an alternative method of determining the total sulfur mass fraction of coal and coke by high-temperature combustion by Coulomb titration.

This document specifies a method for the determination of total carbon, hydrogen and nitrogen in coal and coke by instrumental methods. NOTE This document has been validated for coal only, in accordance with the principles of ISO 5725-1. The suite of samples used in the interlaboratory study (ILS) to determine the precision data did not include coke and therefore there is insufficient data to state precision limits for coke.

This document specifies a method of determining the volatile matter of hard coal and of coke. It is not applicable to brown coals and lignites.

This document specifies a method for the determination of the ash of coal and coke.

This document establishes a practice for the proximate analysis of coal and coke. It is intended for general utilization by the coal industry to provide a basis for comparison of coals and coke and for the determination of fixed carbon.

This document specifies a method for determining the moisture in the general analysis test sample of coke. It can be used for the determination of moisture in blast-furnace coke, foundry-coke and other high-temperature carbonization products.

This document makes reference to ASTM D1412 as a method of determining the moisture-holding capacity of coal.

This document specifies a manual method for the determination of plastometric indices. These indices are the maximum thickness of the plastic layer (Y, mm) and the final contraction value (X, mm). This document is applicable for hard coals with a determined ash level less than 15 % on a dry basis, as described in ISO 11722 and ISO 1171.

This document provides guidance and requirements on the selection of methods used for the determination of trace elements in coal. The trace elements of environmental interest include antimony, arsenic, beryllium, boron, cadmium, chlorine, chromium, cobalt, copper, fluorine, lead, manganese, mercury, molybdenum, nickel, selenium, thallium, vanadium and zinc. The radioactive trace elements thorium and uranium can be added to this list. This document does not prescribe the methods used for the determination of individual trace elements. The analysis of appropriate certified reference materials (CRMs) is essential to confirm the accuracy of any method used (see ISO Guide 33).

This document specifies methods for the determination of thermal stability and thermal fragmentation of coal. It is applicable to brown coal and lignites, anthracites and bituminous coal with a caking index of zero (determined by ISO 15585).

This document specifies a method for the determination of plastometric indices with an automated Sapozhnikov penetration plastometer. These indices are the maximum thickness of the plastic layer, Y, in mm, and the final contraction, X, in mm. This document is applicable to hard coals with a determined ash level of less than 15 % as dry basis as described in ISO 11722 and ISO 1171.

This document specifies the method for determining the reactivity of coal with carbon dioxide (carboxyreactivity). It can be applied to determine the reactivity of coke for the purpose of gasification and combustion.

This document describes methods for the determination of true relative density and the apparent relative density of brown coals and lignites.

This document specifies a method of determining the volatile matter of brown coals and lignites.

This document specifies volumetric methods for the determination of total humic acids and free humic acid of brown coals and lignites.

This document specifies a semi-automatic method for determination of the yield of benzene-soluble extract in brown coals and lignites.

This document specifies a method for the determination of the gross calorific value of a solid mineral fuel at constant volume and at the reference temperature of 25 °C in a combustion vessel calorimeter calibrated by combustion of certified benzoic acid. The result obtained is the gross calorific value of the analysis sample at constant volume with all the water of the combustion products as liquid water. In practice, fuel is burned at constant (atmospheric) pressure and the water is not condensed but is removed as vapour with the flue gases. Under these conditions, the operative heat of combustion is the net calorific value of the fuel at constant pressure. The net calorific value at constant volume can also be used; formulae are given for calculating both values. General principles and procedures for the calibrations and the fuel tests are specified in the main text, whereas those pertaining to the use of a particular type of calorimetric instrument are described in Annexes A to C. Annex D contains checklists for performing calibration and fuel tests using specified types of calorimeters. Annex E gives examples illustrating some of the calculations. Annex F provides guidance around safe use, maintenance and testing of the calorimeter combustion vessel. NOTE Descriptors: solid fuels, coal, coke, tests, determination, calorific value, rules of calculation, calorimetry.

This document establishes a practice for the ultimate analysis of coal and coke and is intended for general utilization by the coal and coke industries to provide a basis for comparison of coals and cokes.

This document specifies a reference method for determining the total sulfur content of hard coal, brown coals and lignites, and coke by the Eschka method.

This document specifies a method of determining the chlorine content of hard coal, brown coals and lignites, and coke using Eschka mixture.

This document specifies a method of determining the volatile matter of brown coals and lignites by the one furnace method.

This document specifies a method for determining the swelling properties of hard coal when heated under standard conditions in a dilatometer.

This document specifies a method of determination of caking index of hard coal. It is applicable to the evaluation of caking power of bituminous coal with random reflectance of vitrinite, Rr, greater than 0,6 % and less than or equal to 1,8 % (>0,6 % and ≤1,8 %).

This document specifies two methods (high temperature combustion and high pressure vessel combustion) for the determination of chlorine in solid mineral fuels. It is applicable to solid mineral fuels. The chlorine in the absorption solution can be determined using different finishes, such as coulometric or potentiometric titration, spectrophotometry or ion chromatography. The method is applicable to determine the chlorine content higher than 0,005 % mass fraction.

This document specifies a gravimetric method of determining the carbon in the mineral carbonates associated with solid mineral fuels. NOTE The result obtained will include any carbon from atmospheric carbon dioxide absorbed by the fuel.