ISO/TC 155 - Nickel and nickel alloys

This document specifies a spectrophotometric method for the determination of the phosphorus content in nickel, ferronickels and nickel alloys between 0,000 5 % (by mass) and 0,05 % (by mass). Arsenic, chromium, hafnium, niobium, silicon, tantalum, titanium and tungsten interfere, but the interferences can be avoided by complexation or volatilization (for chromium). The lowest phosphorus content [0,000 5 % (by mass)] can only be reached in samples with low contents of these interfering elements.

This document lists the International Standards which are currently available for the determination of the chemical composition of nickels, ferronickels and nickel alloys (see Clause 4). It provides details on the range of application and gives the principle of the method described in each International Standard (see Clause 5). Annex A shows graphical representations of the content ranges of the methods listed in this document: Figure A.1 represents the fields of application of the methods available for the three kinds of matrixes; Figure A.2 gives the content ranges of the methods for nickels; Figure A.3 gives the content ranges of the methods for ferronickels; Figure A.4 gives the content ranges of the methods for nickel alloys. Annex B provides a bilingual key of the abbreviated terms used in the figures given in Annex A.

This document specifies a method for the determination of phosphorus, manganese, chromium, copper and cobalt contents in ferronickels, by inductively coupled plasma (ICP) optical emission spectrometry, within the ranges specified in Table 1. This method is applicable to all grades of ferronickels specified in ISO 6501.

This document specifies a molecular absorption spectrophotometric method for the determination of titanium content in nickel alloys. The method is applicable to titanium contents between 0,3 % (mass fraction) and 5,0 % (mass fraction). Molybdenum, if present in the alloy, can cause a high bias in the reported titanium value to the extent of 0,001 % Ti for every 1,0 % Mo. NOTE 1 Evidence exists that extension of this method is possible for titanium contents down to 0,05 % (mass fraction). NOTE 2 Modifications in the general method allow the determination of titanium in alloys containing tungsten and/or tantalum.

This document specifies the technical delivery requirements for the various forms of ferronickel (ingots, pieces and shot) usually supplied for steel making and foundry use.

This document specifies an infrared absorption method after combustion in an induction furnace for the determination of the sulfur content in ferronickels in the range of 0,002 % to 0,12 %. The method is applicable to normal production operations. It uses commercially available equipment, which is calibrated using steel and/or ferronickel certified reference materials (CRMs).

This document specifies an infrared absorption method after combustion in an induction furnace for the determination of the carbon content in ferronickels in the range of 0,004 % to 2,5 %. The method is applicable to normal production operations. It uses commercially available equipment, which is calibrated using steel and/or ferronickel certified reference materials (CRMs).

This document specifies sampling procedures for up to 25 tonnes (metric tons) of refined nickel of the same composition, size and shape and manufactured under similar conditions of production.

This document specifies requirements for nickel and nickel alloy castings. The grades specified represent types of alloys suitable for a broad range of application in a wide variety of corrosive and high temperature environments.

This document specifies an inductively coupled plasma optical emission spectrometric method for the determination of tantalum contents between 0,1 % and 5 % in nickel alloys.

ISO 11437:2018 specifies an electrothermal atomic absorption spectrometric method for the determination of lead in the range of 1 µg/g to 10 µg/g in nickel alloys.

ISO 7529:2017 specifies a potentiometric titration method for the determination of chromium content in nickel alloys which do not contain insoluble carbides and which have a vanadium content less than a mass fraction of 0,2 %. The method is applicable to chromium contents between a mass fraction of 5 % and a mass fraction of 22 %. Vanadium, which can be present as an impurity in the alloy, will give a positive bias interference. However, at a level of a mass fraction of 0,2 %, this bias is equivalent to a mass fraction of 0,068 % chromium, which is about half the reproducibility of the method.

ISO 6283:2017 specifies the designation and chemical composition of grades of refined nickel.

ISO 9725:2017 specifies requirements for nickel and nickel alloy forgings for general purposes.

ISO 8049:2016 defines a method of sampling for analysis of ferronickel lots in the form of shot as specified in ISO 6501 in those cases where lots are constituted either heat by heat or by taking from blended stock. The purpose is to determine the contents of the various elements - either from slugs by physical analysis methods (such as X-ray fluorescence or emission spectral analysis), or - from chips by dry methods (carbon, sulfur) or chemical analysis (other elements).

ISO/TS 18223:2015 describes an inductively coupled plasma atomic emission spectrometric method for the determination of nickel content (mass fraction) between 20,0 % and 80,0 % in nickel alloys. Besides alloys where nickel is the main component regarding its content level, this method may also apply to alloys in which nickel has a content as high as several other elements (Fe, Cr, Co,?) and in which the "main element" cannot be specified.

ISO 7530-1:2015 describes flame atomic absorption spectrometric methods for the determination of cobalt, chromium, copper, iron, and manganese in nickel alloys which can be dissolved in the nitric-hydrochloric acids mixture specified. For each element, the method is applicable to the content range between 0,01 % and 4 %.

ISO 22033:2011 specifies an inductively coupled plasma/atomic emission spectrometric method for the determination of the mass fraction of niobium between 0,1 % and 10 % in nickel alloys.

ISO 11435:2011 specifies an inductively coupled plasma/atomic emission spectrometric method for the determination of the mass fraction of molybdenum between 0,05 % and 20 % in nickel alloys.

The principle of the method specified is dissolving a test portion in acid, aspiring the test solution into a nitrous oxide-acetylene flame of an atomic absorption spectrometer, measuring the absorbance of the resonance line energy from the spectrum of vanadium and comparison with that of calibration solutions at a wavelength of 318,4 nm. The method may be used to determine vanadium contents in the range of 0,05 % (m/m) to 1 % (m/m).

The principle of the method specified is dissolving a test portion in hydrochloric and nitric acids, decomposing resistant boron compounds (e.g. boron nitrides) by fuming the sample solution with phosphoric and sulfuric acids at not less than 290 °C, forming the boron curcumin complex in a buffered acetic acid and sulfuric acid medium, and measuring the absorbance of the test solution in a molecular absorption spectrometer at 543 nm. Applies to nickel and nickel alloys having a total boron content in the range of 4 g/t to 240 g/t.

Silicon content can be determined in the range of 0,2 % (m/m) to 1 % (m/m). The principle is dissolution of a test portion in acid, filtration and aspiration of the test solution into a nitrous oxide-acetylene flame of an atomic absorption spectrometer, combustion of the filter, volatilization of silica, fusion of the residue, dissolution of the melt in dilute acid, aspiration of this second solution into another such flame, measurement of the absorbance of the resonance line energy from the spectrum of aluminium and comparison with that of calibration solutions at 309,3 nm.

Silicon content can be determined in the range of 0,2 % (m/m) to 1 % (m/m). The principle is dissolution of a test portion in acid, aspiration of the test solution into a nitrous oxide-acetylene flame of an atomic absorption spectrometer, measurement of the absorbance of the resonance line energy from the spectrum of silicon and comparison with that of calibration solutions at 251,6 nm.

Phosphorus content can be determined in the range of 0,001 % (m/m) to 0,025 % (m/m). Cr(III) and silica cause interference which is eliminated. The principle is dissolution of a test portion in a mixture of nitric and hydrochloric acids, fuming with sulfuric acid, oxidation of Cr(III) to Cr(VI), precipitation of Fe(III) phosphate and redissolution of the precipitate, addition of boric, tartaric and sulfamic acids, formation and extraction of molybdophosphoric acid, reduction of the heteropoly acid to molybdenum blue and back-extraction into an aqueous phase, measurement of the absorbance of the aqueous solution at 700 nm.

Applies to ferronickel lots in ingot or piece form with a view to obtaining a representative laboratory sample for the determination of the chemical composition of the lot. A choice is to be made between a first procedure that can be applied at the producer's plant during casting or a second procedure that can be applied to lots as delivered at the buyer's premises. Includes two alternatives for sample taking (drilling and milling). Each party is entitled to participate in sampling operations.

Applies to nickel contents in the range 15 to 60 % (m/m). Specifies principle, reagents, apparatus and samples, procedure, expression of results and test report. Annex A is provided for the determination of nickel in combined filtrates by atomic absorption spectrometry. Annex B gives a statistical report of interlaboratory tests.

Applies to the determination of the given elements of high purity, refined, wrought and cast nickel within the ranges specifies in table 1. This method is applicable to the indipendent determination of any one or more of the elements listed. Annex A gives an alternative method for preparation of nickel nitrate solution for electrothermal atomic analysis, and annex B contains a statistical report of interlaboratory tests.

Applies to refined, wrought and cast nickel within the ranges specified in table 1. The method is applicable to the independent determination of any one or more of the elements listed. The lower level for iron can be extended to less than 0,0025 % (m/m) provided a special standard solution is prepared. The upper limit for the determination of cobalt and copper can be raised to 2 % (m/m) by a minor modification to the method. For potential interferences, see clause 10.

Applies to cobalt contents in the range 0,025 to 2,5 % (m/m). Specifies principle, reagents, apparatus, sampling and samples, procedure, expression on results, special cases and test report.

Specifies a method for the determination of silicon in ferronickel in the range 0,2 to 4,0 % (m/m). Gives principle, reagents, apparatus, sampling and samples, procedure, expression of results and test report.

ISO 22725:2007 specifies an inductively coupled plasma atomic emission spectrometric method for the determination of the mass fraction of tantalum between 0,1 % and 5 % in nickel alloys.

ISO 22033:2005 specifies an inductively coupled plasma atomic emission spectrometric method for the determination of the mass fraction of niobium between 0,1 % and 10 % in nickel alloys.

ISO 11435:2005 specifies an inductively coupled plasma atomic emission spectrometric method for the determination of the mass fraction of molybdenum between 0.05 % and 20 % in nickel alloys.

Specifies a gravimetric method for the determination of nickel content of nickel oxide and partially reduced nickel oxide in the range of 70 % to 95 % (m/m).

Specifies the designation and chemical composition of commercially available grades of refined nickel.

Specifies an electrothermal atomic absorption spectrometric method for the determination of lead in the range of 0,5 g/tonne to 10,0 g/tonne in nickel alloys. Gives the general requirements concerning the apparatus, sampling, dissolution of the test sample, atomic absorption measurements, calculation and test report.

Specifies electrothermal atomic absorption methods for the determination of trace elements in nickel alloys, in the concentration ranges given in clause 1 of other parts of ISO 11437. Gives in annex B typical compositions of some nickel alloys. Specifies the general requirements for analysis by electrothermal atomic absorption spectrometry, preparation and dissolution of the test sample, method of calculation and the procedures used for the evaluation of the repeatability and reproducibility of the individual methods specified in other parts of ISO 11437.

The principle of the method specified is dissolution of a test portion in nitric acid, measurement of the absorption of the resonance line energy from the spectrum of tin in the test solution at a wavelength of 286,3 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer, calibration by the standard additions method described in ISO 11438-1. Applies to tin contents in the range of 1,0 g/t to 10,0 g/t in ferronickel.

Specifies the general requirements for analysis by electrothermal atomic absorption spectrometry, preparation and dissolution of the test sample, general procedure, method of calculation and the procedures used for the evaluation of the repeatability and reproducibility of the individual methods specified in the other parts of ISO 11438.

The principle of the method specified is dissolution of a test portion in nitric acid, measurement of the absorption of the resonance line energy from the spectrum of thallium in the test solution at a wavelength of 276,8 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer, calibration by the standard additions method described in ISO 11438-1. Applies to thallium contents in the range of 0,3 g/t to 1,0 g/t in ferronickel.

The principle of the method specified is dissolution of a test portion in nitric acid, measurement of the absorption of the resonance line energy from the spectrum of tellurium in the test solution at a wavelength of 214,3 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer, calibration by the standard additions method described in ISO 11438-1. Applies to tellurium contents in the range of 0,3 g/t to 2,0 g/t in ferronickel.

The principle of the method specified is dissolution of a test portion in nitric acid, measurement of the absorption of the resonance line energy from the spectrum of lead in the test solution at a wavelength of 283,3 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer, calibration by the standard additions method described in ISO 11438-1. Applies to lead contents in the range of 1,0 g/t to 5,0 g/t in ferronickel.

The principle of the method specified is dissolution of a test portion in nitric acid, measurement of the absorption of the resonance line energy from the spectrum of silver in the test solution at a wavelength of 328,1 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer, calibration by the standard additions method described in ISO 11438-1. Applies to silver contents in the range of 1,0 g/t to 6,0 g/t in ferronickel.

The principle of the method specified is dissolution of a test portion in nitric acid, measurement of the absorption of the resonance line energy from the spectrum of indium in the test solution at a wavelength of 325,6 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer, calibration by the standard additions method described in ISO 11438-1. Applies to indium contents in the range of 0,5 g/t to 2,5 g/t in ferronickel.

The principle of the method specified is dissolution of a test portion in nitric acid, measurement of the absorption of the resonance line energy from the spectrum of antimony in the test solution at a wavelength of 217,6 nm by an atomic absorption spectrometer fitted with a graphite furnace electrothermal atomizer, calibration by the standard additions method described in ISO 11438-1. Applies to antimony contents in the range of 1,0 g/t to 5,0 g/t in ferronickel.

The principle of the method specified is dissolving a test portion in hydrochloric and nitric acids, removing hydrochloric acid and nitric acid by evaporation to fumes in the presence of sulfuric acid, forming the titanium diantipyrylmethane complex, measuring the absorbance of the test solution at a wavelength of 390 nm. The method may be used to determine titanium contents in the range of 0,3 % (m/m) to 5,0 % (m/m). Evidence exists that extension of this method is possible for titanium contents down to 0,05 % (m/m); modifications allow to determine titanium in alloys containing tungsten and/or tantalum.

Specifies ordering information, requirements for forgings heat treated by the manufacturer and forgings to be heat treated by the purchaser, sampling, test procedures, marking, purchaser or third party inspection, declaration of conformity. Annex A gives a list of ISO methods of analysis.