ISO/TC 102/SC 2 - Chemical analysis

This document specifies a performance-based method for the chemical analysis of natural and processed iron ores by fused bead wavelength and energy dispersive X-ray fluorescence (XRF). It is applicable to all elements of interest when adequate calibrations have been established.

This document specifies a photometric titration method using EDTA for the determination of the total iron content of iron ores. This method is applicable to a concentration range of a mass fraction of 37,00 % to 72,00 % of total iron in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

This document specifies a potentiometric titration method for the determination of total iron content of iron ores, using potassium dichromate as titrant after reduction of the iron(III) by tin(II) chloride and titanium(III) chloride. The excess reductant is then oxidized by potassium dichromate solution. This method is applicable to total iron contents between a mass fraction of 29,04 % and a mass fraction of 72,02 % in natural iron ores and iron ore concentrates and agglomerates including sinter products.

This document specifies two titrimetric methods, free from mercury pollution, for the determination of total iron content in iron ores, using potassium dichromate as titrant after reduction of the iron(III) by tin(II) chloride and titanium(III) chloride. The excess reductant is then oxidized by either dilute potassium dichromate (Method 1) or perchloric acid (Method 2). Both methods are applicable to a concentration range of 30 % mass fraction to 72 % mass fraction of iron in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 15633:2017 specifies a flame atomic absorption spectrometric method for the determination of the nickel mass fraction of iron ores. This method is applicable to mass fractions of nickel between 0,001 % and 0,10 % in natural iron ores, iron ore concentrates and agglomerates including sinter products. This method is not appropriate for referee purposes.

ISO 22682:2017 specifies a method for the determination of phosphorus, vanadium, titanium, copper, nickel, chromium, barium and cobalt in iron ores, by inductively coupled plasma atomic emission spectrometry (ICP-AES).

ISO 10204:2017 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of magnesium in iron ores. This method is applicable to mass fractions of magnesium between 0,010 % and 2,00 % in natural iron ores, iron ore concentrates, and agglomerates, including sinter products.

ISO/TR 9686:2017 specifies a method for the determination of the mass fraction of carbon and/or sulfur in direct reduced iron by infrared measurement after high-frequency combustion. This method is applicable to mass fractions of carbon between 0,05 % and 2,5 %, and/or mass fractions of sulfur between 0,001 % and 0,05 % in direct reduced iron.

ISO/TR 4688-1:2017 describes a flame atomic absorption spectrometric method for the determination of the mass fraction of aluminium in iron ores. This method is applicable to mass fractions of aluminium between 0,1 % and 5,0 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 10203:2017 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of calcium in iron ores. This method is applicable to mass fractions of calcium between 0,010 % and 8,00 % in natural iron ores, iron ore concentrates, and agglomerates, including sinter products.

ISO 13312:2017 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of potassium in iron ores. This method is applicable to mass fractions of potassium between 0,002 5 % and 0,52 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 13313:2017 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of sodium in iron ores. This method is applicable to mass fractions of sodium between 0,002 5 % and 0,50 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 4689-3:2017 specifies a combustion/infrared method, using a high-frequency induction furnace, for the determination of the sulfur content of iron ores. This method is applicable to sulfur contents between 0,002 % (mass fraction) and 0,25 % (mass fraction) in natural iron ores, iron ore concentrates and agglomerates, including sinter products. The method is not applicable to iron ores containing more than 1,0 % (mass fraction) of combined water. The apparatus, of which the metal filter is equipped with a heating device, can be applied to iron ores containing less than 3,0 % (mass fraction) of combined water.

ISO 4689-2:2017 specifies a combustion/titration method for the determination of the sulfur content of iron ores. This method is applicable to sulfur contents between 0,002 % (mass fraction) and 0,25 % (mass fraction) in natural iron ores, iron ore concentrates, and agglomerates, including sinter products. The results are not affected by the presence of fluoride.

ISO 16878:2016 specifies a titrimetric method for the determination of the metallic iron content of reduced iron ores. This method is applicable to a concentration range of 57,5 % mass fraction to 90,5 % mass fraction of the metallic iron. NOTE The term "metallic iron" means those forms of iron not bonded to oxygen or not present as pyrite.

ISO/TR 18231:2016 describes methods of test that can be applied to wavelength dispersive X-ray fluorescence (WD-XRF) spectrometers to ensure that the spectrometers are functioning in a manner that allows precise analyses to be made. The tests outlined are designed to measure the errors associated with the operation of certain parts of the spectrometer. They are not designed to check every part of the spectrometer but only those parts that may be the common sources of error. It is assumed that the performance of the instrument has been optimized according to the manufacturer's instructions. For all tests, the two-theta angle should be carefully set for the line being measured. The pulse height window should be set according to the manufacturer's instructions and should have a broad setting which may also include the escape peak for gas proportional counters. The instrument and detector gas environment should be as specified by the manufacturer, as should the power supply to the instrument. NOTE Where no distinction has been made, it is assumed that a test is applicable to both sequential and simultaneous spectrometers.

ISO/TR 18336:2016 specifies recommended quality control procedures for XRF laboratories operating within the iron ore industry.

ISO/TR 16043:2015 sets out a wavelength dispersive X-ray fluorescence procedure for the determination of chlorine in iron ores. The method is applicable to a concentration range of 0,027 % to 1,15 % of chlorine in iron ores regardless of mineralogical type. It is not intended that this method be used for the purpose of trade in iron ores due to the precision of the method.

ISO/TR 18230:2015 describes a gravimetric method for the determination of the loss in mass of non-oxidized iron ores, when ignited at 1 000 °C. This method is applicable to a concentration range of a mass fraction of −3,0 % to 7,0 % loss on ignition in natural iron ores, iron ore concentrates and agglomerates, and sinters. The method is not applicable to the following: a) processed ores containing metallic iron (direct reduced iron); b) natural or processed ores in which the sulfur content is higher than a mass fraction of 0,2 %; c) internationally traded ores with combined water greater than 2,5 %. NOTE 1 Loss on ignition can be used as an estimate of combined water. NOTE 2 This method is intended for in-house use and is not intended for referee purposes.

ISO 15634:2015 specifies a flame atomic absorption spectrometric method for the determination of the chromium content of iron ores. This method is applicable to chromium contents between 0,001 6 % and 0,1 % (mass fractions) in natural iron ores, iron ore concentrates, and agglomerates including sinter products.

ISO 11536:2015 specifies a gravimetric method for the determination of the loss in mass of fully-oxidized iron ores, when ignited at 1 000 °C. This method is applicable to a concentration range of 1,0 % (m/m) to 10,0 % (m/m) loss on ignition in natural iron ores, iron ore concentrates and agglomerates. The method is not applicable to the following: a) Processed ores containing metallic iron (direct reduced iron); b) Natural or processed ores in which the sulfur content is higher than 0,2 % (m/m); c) Natural or processed ores in which the content of partially-oxidized iron is more than 1,0 % (m/m).

ISO 17992:2013 specifies a hydride generation atomic absorption spectrometric method for the determination of the arsenic content of iron ore. ISO 17992:2013 is applicable to mass fractions of arsenic between 0,000 66 % and 0,020 15 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 11533:2009 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of cobalt in iron ores. This method is applicable to a mass-fraction range of 0,000 7 % to 0,06 % of cobalt in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 9683-2:2009 specifies two flame atomic absorption spectrometric methods for the determination of the mass fraction of vanadium in iron ores. Method 1 is applicable to mass fractions of vanadium between 0,004 % and 0,06 %, and Method 2 to mass fractions of vanadium between 0,06 % and 0,5 %, in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

SO 9682-1:2009 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of manganese in iron ores. This method is applicable to a mass-fraction range of 0,01 % to 2,5 % of manganese in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 4691:2009 specifies a spectrophotometric method using diantipyrylmethane for the determination of the mass fraction of titanium in iron ores. ISO 4691:2009 is applicable to a mass-fraction range of 0,02 % to 4,0 % of titanium in natural iron ores, and iron ore concentrates and agglomerates including sinter products.

ISO 9517:2007 specifies an ion-selective electrode method for the determination of the mass fraction of water-soluble chloride in iron ores. This method is applicable to a mass-fraction range of 0,007 % to 0,1 % of water-soluble chloride in natural iron ores, concentrates and agglomerates, including sinter products.

ISO 16042:2007 describes recommended procedures for the use of CRMs that have been prepared and certified in accordance with ISO 11459. Such CRMs are used by laboratories to carry out the trueness tests as specified in the various International Standards for the chemical analysis of iron ores, to verify the analysis of shipment samples and the ongoing reliability of analytical results.

ISO 9682-2:2006 specifies a spectrophotometric method using sodium periodate for the determination of the mass fraction of manganese in iron ores. This method is applicable to a mass-fraction range of 0,02 % to 8 % of manganese in natural iron ores, and iron ore concentrates and agglomerates, including sinter products.

ISO 11535: 2006 specifies a method for the determination of aluminium, calcium, phosphorus, magnesium, manganese, silicon and titanium in iron ores by inductively coupled plasma atomic emission spectrometry.

ISO 5418-1:2006 specifies a 2,2'-biquinolyl spectrophotometric method for the determination of copper in iron ores. This method is applicable to mass fractions of copper between 0,005 % and 0,77 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 9683-1:2006 specifies a spectrophotometric method using N-benzoyl-phenylhydroxylamine (BPHA) for the determination of the mass fraction of vanadium in iron ores. This method is applicable to mass fractions of vanadium between 0,005 and 0,5 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 5418-2:2006 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of copper in iron ores. This method is applicable to a mass-fraction range of 0,004 % to 0,8 % of copper in natural iron ores, and iron ore concentrates and agglomerates, including sinter products.

ISO 11534:2006 specifies a flame atomic absorption spectrometric method for the determination of the mass fraction of tin in iron ores. This method is applicable to mass fractions of tin between 0,001 % and 0,015 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 2496:2006 specifies the following four test methods for the determination of the hygroscopic moisture content of test samples: Method 1 -- Gravimetric method; Method 2 -- Karl Fischer volumetric method; Method 3 -- Karl Fischer coulometric method; Method 4 -- Mass-loss method. Any of these methods is applicable wherever the analytical value of a chemical constituent is to be calculated to a dried sample basis in the following ore types. Processed ores containing metallic iron (direct reduced iron). Natural or processed ores in which the sulfur content is greater than 0,2 % (mass fraction). Natural or processed ores in which the combined water is greater than 2,5 % (mass fraction). Any of these methods is applicable to a concentration range of 0,05 % (mass fraction) to 4,5 % (mass fraction) hygroscopic moisture.

ISO 2597-1:2006 specifies a titrimetric method for the determination of the total iron content of iron ores, using potassium dichromate after reduction of the trivalent iron by tin(II) chloride. The method is applicable to total iron contents between 30 % (mass fraction) and 72 % (mass fraction) in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

ISO 7764:2006 specifies a method for the preparation of predried test samples of natural iron ores, and iron ore concentrates and agglomerates, including sinter products, which are to be used for the determination of analytical values of constituents on a dry basis. The method is not applicable to the following types of ores: processed ores containing metallic iron (direct-reduced iron); natural or processed ores in which the mass fraction of sulfur is higher than 0,2 %; natural or processed ores in which the content of combined water is higher than 2,5 % by mass.

ISO 5416:2006 specifies a titrimetric method for the determination of the mass fraction of metallic iron in reduced iron ores (direct reduced iron: DRI). This method is applicable to mass fractions of metallic iron between 15 % and 95 % in DRI.

ISO 9516-1:2003 sets out a wavelength dispersive X-ray fluorescence procedure for the determination of iron, silicon, calcium, manganese, aluminium, titanium, magnesium, phosphorus, sulfur, potassium, tin, vanadium, chromium, cobalt, nickel, copper, zinc, arsenic, lead and barium in iron ores. The method has been designed to cope with iron ores having high ignition losses. The method is applicable to iron ores regardless of mineralogical type.

ISO 2599:2003 specifies a titrimetric method for the determination of the phosphorus content of iron ores, using hexaammonium heptamolybdate (ammonium molybdate). This method is applicable to a concentration range of 0,10 % (m/m) to 5,0 % (m/m) of phosphorus in natural iron ores, and iron ore concentrates and agglomerates including sinter products. This International Standard provides a quality control method for the determination of phosphorus by titration, however, the method cannot be used for referee purposes.

Recommends procedures for iron ore dissolution using either acid digestion or alkali fusion. Deals with the assessment of the advantages and disadvantages of the two procedures.

The method is based on decomposition of the test portion by 1) sintering with sodium peroxide and treatment with hydrochloric and perchloric acids and treatment with dilute nitric acid, or 2) treatment with hydrochloric, nitric and perchloric acids, evaporation, filtration of silica with any residue, fusion with sodium carbonate and dissolution in hydrochloric and perchloric acids, in both cases evaporation of the solution, filtration of the precipitated silica, ignition, and weighing, treatment of the ignited residue with hydrofluoric and sulfuric acid, ignition, and reweighing. Applies to silicon contents between 1 % and 15 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

The method is based on decomposition of the test portion by fusion with sodium tetraborate and treatment with dilute nitric acid, addition of ammonium molybdate to convert silicate into a molybdatosilicate complex, reduction to molybdenum blue with ascorbic acid, and spectrophotometric measurement of the absorbance of the molybdenum blue complex at a wavelength of approximately 600 nm. Applies to silicon contents between 0,1 % and 5,0 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products, especially for ores containing fluorine.

The method is applicable to phosphorus contents between 0,003 % (m/m) and 2 % (m/m) in natural iron ores, iron ore concentrates and agglomerates, including sinter products. The presence of arsenic, barium or titanium does not affect the result.

The specified method applies to nickel and/or chromium contents between 0,003 % (m/m) and 0,1 % (m/m) in natural iron ores, iron ore concentrates and agglomerates, including sinter products.

Is applicable to natural and processed iron ores containing from 1 % to 25 % acid-soluble iron(II) and only traces of metallic iron. Is limited for use in conjunction with the reducibility test methods. Is not applicable to ores containing more than 0,3 % (m/m) sulfur (as sulfide) and/or 5 % free carbon. Specifies principle, reagents, apparatus, sampling and samples, procedure, expression of results and test report. Includes three annexes.

The method ist applicable to a concentration range of 0,0001 to 0,1 % (m/m) (1 bis 1000 /g) of arsenic in natural iron ores, and iron ore concentrates and agglomerates including sinter products. Specifies principle, reagents, apparatus, sampling and samples, procedure, expression of results, and test report. Includes three annexes. A figure shows the arsenic distillation apparatus.