ISO TR 9769:2018 download

05-20-2021 comment

ISO TR 9769:2018 download.Steel and iron – Review of available methods of analysis.
I Scope
ISO TR 9769 gives guidelines for the determination of the chemical composition of steel and iron by reference to published International Standards, including their range of application and principles of the methods,
Graphical representation olthe precision data precison data for the methods is given In AaneyA. The list of International Standards Is summarized In Annex B.
2 Normative references
There are no normative references in ISO TR 9769.
3 Terms and definitions
For the purposes of ISO TR 9769, the following terms and definitions apply.
ISO and IEC maintain termlnologlcal databases for use In standardization at the following addresses:
— ISO Online browsing platform: available at
— IEC Electropedia: available at
3.1
routine method
method calibrated against reference materials, certified reference materials or against standard solutions commercially available that is widely used for control purposes (day-to-day analysis)
4 International Standards for determining the chemical composition of steel and
Iron, their range of application and principles of the methods
4.1 Mono-elemental methods
4.1.1 AluminIum, Al
Document: ISO 9658:1990, Steel — Determination of aluminium content — Flame atomic absorption spectrometrc method.
Range of application:
— determination of acid-soluble and/or total aluminium contents between a mass fraction of 0.005% and a mass fraction oF 0,20 % in non-alloyed steel.
Principle of the method:
a) dissolution of a test portion in dilute hydrochloric and nitric acids;
b) fusion of the acid-insoluble material with a mixture of orthoboric acid and potassium carbonate;
c) spraying of the solution into a dinitrogen monoxide-acetylene flanw;
4.1.2 Antimony, Sb
Document: ISO 10698:1994, Steel — Determination of antimony content — Electrothermal atomic absorption spectromeeric method.
Range of application:
— determination of the antimony content between a mass fraction of 0,0005% and a mass fraction of 0,0 10 % in steel.
Principle of the method:
a) dissolution of a test portion in hydrochloric and nitric acids and dilution of the solution to a known volume;
b) introduction of a known volume of the solution into an electrothermal atomizer of an atomic absorption spectrometer;
c) measurement of the atomic absorption of the 217,6 nm spectral resonance line energy emitted by an antimony lamp, using background correction;
d) calibration by the standard additions technique.
4.1.3 Arsenic, As
Document: ISO 17058:2004, Steel and iron — Determination of arsenic content — Spectrophotometric method.
Range of application:
— determination of the arsenic content between 0,000 5 % (mass fraction) and 0,10 % (mass fraction) in steel and iron.
Principle of the method:
a) dissolution of a test portion in a hydrochloric acid and nitric acid mixture;
b) prolonged heating with sulfuric acid until white fumes are given off;
c reduction of arsenic in the nresence of hvdrazine sulfate and notassium bromide. then senaration by distillation as the trivalent chloride, absorbed in the nitric acid solution, in which the As(lll) is oxidized back to the pentavalent state As(V);
d) formation of the molybdenum blue complex between ammonium molybdate and arsenic, which is reduced by hydrazine sulfate;
e) spectrophotometric measurement at a wavelength of approximately 840 nm.
4.1.4 Boron,B
4.1.4.1 Document: ISO 10153:1997, Steel — Determination of boron content — Curcumin spectrophotometric method.
Range of application:
— determination of the boron content between a mass fraction of 0,000 1 % and a mass fraction of 0,000 5 % only in unalloyed steel, and between a mass fraction of 0,000 5 % and a mass fraction of
0,0 12 % in steel.
4.1.4.2 Document: ISO 13900:1997, Steel — Determination of boron content — Curcumin spectrophotometric method after distillation.
Range of application:
— determination of the boron content between a mass fraction of 0,000 05 % and a mass fraction of 0,00 1 0 % in steel.
Principle of the method:
a) dissolution of a test portion in hydrochloric and nitric acids;
b) decomposition of boron compounds (nitrides etc.) with orthophosphoric and sulfuric acids at a temperature of 290 °C;
c) distillation of the solution after the addition of methanol and collection of methylborate in a receiver containing sodium hydroxide solution;
d) evaporation of the solution to dryness; formation of a coloured complex between orthoboric acid and curcumin in a methanol medium;
e) spectrophotometric measurement at a wavelength of about 550 nm.
4.1.5 Calcium, Ca
4.1.5.1 Document: ISO 10697-1:1992, Steel — Determination of calcium content by flame atomic absorption spectrometry — Part 1: Determination of acid-soluble calcium content.
Range of application:
— determination of acid-soluble calcium content between a mass fraction of 0,000 5 % and a mass fraction of 0,003 % in steel.
4.1.6 Carbon, C
4.1.61 Document: ISO 9556:1989, Steel and iron — Determination of total carbon content — lnjrared absorption method after combustion in an induction furnace.
Range of application:
— determination of the total carbon content between a mass fraction of 0,003 % and a mass fraction of 4,5 % in steel and iron.
Principle of the method:
a) combustion of a test portion with accelerator at a high temperature in a high-frequency induction furnace in a current of pure oxygen; transformation of carbon into carbon dioxide and/or carbon monoxide;
b) measurement by infrared absorption of the carbon dioxide and/or carbon monoxide carried by a current of oxygen.
4.1.6.2 Document: ISO 15349-2:1999, Unalloyed steel — Determination of low carbon content — Part 2:
Infrared absorption method after combustion in an induction furnace (with preheating).
Range of application:
— determination of the carbon contents between a mass fraction of 0,000 3 % and a mass fraction of 0,010 % in unalloyed steel.
Principle of the method:
a) preheating of a test portion at low temperature and combustion of a test portion with accelerator at a high temperature in an induction furnace in a current of pure oxygen; transformation of carbon into carbon dioxide and/or carbon monoxide;
b) measurement of infrared absorption of the carbon dioxide or carbon dioxide/carbon monoxide evolved from steel and carried by a current of pure oxygen;
4.1.7 Chromlum,Cr
4.1.7.1 Document: ISO 4937:1986, Steel and iron — Determination of chromium content — Potentiametric or visual titration method.
Range of apphcation:
— determination of chromium contents between a mass fraction of 0,25% and a mass fraction of 35 % in steel and iron.
NOTE If vanadium is present, the visual titration Is applicable only to test portions containing less than 3 mg of vanadium.
Principle of the method:
a) dissolution of a test portion with appropriate acids;
b) oxidation of chromium in an acid medium to chromium(Vl) by ammonium peroxydisulfate in the presence of silver sulfate; reduction of manganese(VlI) by hydrochloric acid;
c) reduction of chromium(VI) by ammonium iron(lI) sulfate standard solution;
d) in the case of potentiometric detection, determination of the equivalence point by measurement of the potential variation when the ammonium iron(ll) sulfate standard solution is being added;
e) in the case of visual detection, titration of the excess ammonium iron(ll) sulfate by potassium permanganate standard solution, which also acts as the indicator.
4.1.7.2 Document: ISO 10138:1991, Steel and iron — Determination of chromium content — Flame
atomic absorption spectrometric method.
Range of application:
— determination of chromium contents between a mass fraction of 0,002 % and a mass fraction of 2,0 % in non-alloy and low-alloy steels and iron.
4.1.7.3 Document: ISO 15355:1999, Steel and iron — Determination of chromium content — indirect titration method.
Range of application:
— determination of chromium content between a mass fraction of 1 % and a mass fraction of 35% In steel and iron.
Vanadium contents in steel and iron should be less than a mass fraction of 1 % for chromium contents higher than a mass fraction of 10 % and less than a mass fraction of 0,2 % for chromium contents less than a mass fraction of 10 %.
Principle of the method:
a) fusion of the sample with sodium peroxide followed by acidification with sulfuric acid;
b) oxidization of chromium(IlI) to dichromate with peroxodisulfate using silver as a catalyst;
c) reduction of the dichromate with an excess of a solid iron(lI) salt and potentiometric back titration of the excess with a dichromate solution;
d) any interference from vanadium is corrected mathematically.
4.1.8 Cobalt, Co
4.1.8.1 Document: ISO 11652:1997, Steel and iron — Determination of cobalt content— Flame atomic absorption spectrometric method.
Range of applicat ion:
— determination of the cobalt content between a mass fraction of 0,003 % and a mass fraction of 5,0% in steel and iron.
Principle of the method:
a) dissolution of a test portion in hydrochloric, nitric and perchioric acids;
b) spraying of the solution into an air-acetylene flame;
4.1.8.3 Document: ISO 13898-4:1997, Steel and iron — Determination of nickel, copper and cobalt contents — Inductively coupled plasma atomic emission spectrometric method — Part 4: Determination of cobalt content.
Range of application:
— determination of cobalt content between a mass fraction of 0,00 1 % and a mass fraction of 0,10 % in unalloyed steel and unalloyed iron.
Principle of the method:
a) dissolution of a test portion in a mixture o[hydrochloric and nitric acids and dilution oithe solution to known volume;
b) if necessary. addition of scandium or yttrium as internal standard;
c) nebulization of the solution into an inductively coupled plasma atomic emission spectrometer (ICrAES) and measurement of the intensity of the emitted light from each element, or with emitted light from scandium or yttrium, simultaneously; examples of the analytical lines are given in ISO 13898-1:1997, Table 2.
4.1.9 Copper, Cu
4.1.9.1 Document: ISO 4943:1985, Steel and cast iron — Determination of copper content — Flame atomic absorption spectrometric method.
Range of application:
— determination of copper contents in the range of a mass fraction of 0,004 % to a mass fraction of 0.5 % in steel and cast iron.
Principle of the method:
a) dissolution of a test portion in a mixture of hydrochloric, nitric and perchioric acids;
b) spraying of the solution into an air-acetylene flame; spectrometric measurement of the atomic
4.1.8.3 Document: ISO 13898-4:1997, Steel and iron — Determination of nickel, copper and cobalt contents — Inductively coupled plasma atomic emission spectrometric method — Part 4: Determination of cobalt content.
Range of application:
— determination of cobalt content between a mass fraction of 0,00 1 % and a mass fraction of 0,10 % in unalloyed steel and unalloyed iron.
Principle of the method:
a) dissolution of a test portion in a mixture o[hydrochloric and nitric acids and dilution oithe solution to known volume;
b) if necessary. addition of scandium or yttrium as internal standard;
c) nebulization of the solution into an inductively coupled plasma atomic emission spectrometer (ICrAES) and measurement of the intensity of the emitted light from each element, or with emitted light from scandium or yttrium, simultaneously; examples of the analytical lines are given in ISO 13898-1:1997, Table 2.
4.1.9 Copper, Cu
4.1.9.1 Document: ISO 4943:1985, Steel and cast iron — Determination of copper content — Flame atomic absorption spectrometric method.
Range of application:
— determination of copper contents in the range of a mass fraction of 0,004 % to a mass fraction of 0.5 % in steel and cast iron.
Principle of the method:
a) dissolution of a test portion in a mixture of hydrochloric, nitric and perchioric acids;
b) spraying of the solution into an air-acetylene flame; spectrometric measurement of the atomic
4.1.10.3 Document: ISO 10278:1995, Steel — Determination of manganese content — Inductively coupled plasma atomic emission spectrometric method.
Range of application:
— determination of the manganese content between a mass fraction of 0,002 % and a mass fraction of 1,5 % in unalloyed steels.
Principle of the method:
a) dissolution of a test portion in a mixture of hydrochloric and nitric acids and dilution of the solution to a known volume;
b) if necessary, addition of scandium or yttrium as an internal standard;
c) nebulization of the solution into an ICP-AES and measurement of the intensity of the emitted light from manganese at 257,61 nm and, optionally, emitted light from scandium at 361,38 nm or yttrium at 371,03 nm. simultaneously.
4.1.10.4 Document: ISO 18632:2018, Alloyed steels — Determination of manganese — Potentiometric or
visual titration method.
Range of application:
— determination of the mass fraction of manganese between 2% and 25 % in alloyed steels.
NOTE Vanadium and cerium interfere with the determination, lithe mass fraction of cerium in the sample Is less than 0,01 %, or the mass fraction of vanadium in the sample is less than 0,005 %, the interference Is negligible, otherwise theoretical corrections are necessary.
Principle of the method:
a) dissolution of a test portion in appropriate acids;
b) addition of phosphoric acid; oxidation of manganese to manganese(lll) in phosphoric acid medium with ammoniurn nitrate;
Principle of the method:
a) dissolution of a test portion In an appropriate mixture of acids and decomposition of the carbides by oxidation:
b) quantitatwe formation of a coloured compound of molybdenum. in the presence of thiocyanate. iron(Il) and/or copper(lI) ions and extraction of this compound using butyl acetate:
c) spectrophotometric measurement of the coloured compound at a wavelength of about 470 nm.
4.1.11.2 Document: 1SO/TS 13899-1:2004, Steel— DetermvnaUon of ?4o, Nb and Wcontentsu, alloyed steel — Inductively coupled plasma atomic emission spectrometnc method — Part 1: Determination of Mo content,
Range of application:
— determination of molybdenum content between a mass Fraction of 0.03 % and a mass fraction of 8,5% in steel.
Principle of the method:
a) dissolution of a test portion in a mixture of hydrochloric, nitric and phosphoric acid and fuming with a mixture of phosphoric and perchloric acids:
b) addition of hydrofluoric acid and, if necessary, an Internal reference element and dilution of the solution to known volume;
c) nebulizatinn of the solution into an ICP-AES and measurement of the intensity of the emitted light from molybdenum, or with emitted light from the internal reference element, simultaneously.
NOTE 1 The method uses a calibration graph based ona very close matrix matchingof the calibration solutions to the sample and dose bracketing of the contents around the approximate Loncentratlon of molybdenum In the sample to be analysed. The concentrations of all elements In the sample have to be, therefore, approximately known. If the concentrations are not known, the sample has to be analysed by some semi-quantitative method.
NOTE 2 The advantage with this procedure Is that all possible Interferences from the matrix areautomatically compensated, which results In high accuracy. This is most important for spectral interferences, which can be severe in very highly alloyed steels. However, alt possible interferences have to be kept on a minimum level. Therefore, It is essential that the spectrometer used meets the performance criteria specified In the method for the selected analytical lines,
4.1.12 Nickel,Ni
4.1.12.1 Document: ISO 4940:1985. Steel and cost iron — Determination of nickel content — Flame atomic absorption spectrometric method.
Range of application:
— determination of nickel contents in the range of a mass traction of 0.002 % to a mass fraction of 0,5% in steel and cast iron.
Principle of the method:
a) dissolution of a test portion In a mixture of appropriate acids foLlowed by evaporation to fuming with perchioric acid:
b) spraying of the solution into an air-acetylene flame; spectrometric measurement of the atomic absorption of the 352.5 nm spectral line emitted by a nickel hollow cathode lamp.
NOTE I With some instruments it is not possible to obtain sufficient sensiLivity at the wavelength of 352,5 nm for low concentrations of nickel mar the botom end of the application range. In such cases, the alternative wavelength of 232,0 nm is used.
NOTE 2 At the wavelength of 352,5 nm, the signal.to.noise ratio is higher than at a wavelength of 232,0 nm In general. use ol the 352.5 nm line will give better reproducibility.
4.1.12.2 Document: ISO 4938:2016. Steel and iron — Determination of nickel content — Gravimetrk or tltrimetric method.
Range olapphcat ion:
— determination of nickel contents from a mass fraction of 1 % to a mass fraction of 30 % In steel and iron.
Principle of the method:
a) dissolution of a test portion with appropriate acids;
b) precipitation of the nickel as nickcl.dimethylglyoxime;
— cobalt, if present, is oxidized by potassium hexacyanoferrate(llI):
— copper. ii present with cobalt, preferably Is removed by controlled potential electrolysis;
c) acid dissolution of the precipitate and filtration of the solution, followed by a second precipitation of the nickel as nickel dlmethylglyoxlme;
d) in the case of the gravimetric determination, weighing the dried dimethyiglyoxime precipitate:
e) in the case of the titri metric determination, acid dissolution of the precipitate. addition of excess EDTA.Na2 solution and back titration of the excess EDTA.Na2 by zinc solution using xylenol orange as an lnd1cator
f) In both cases, determination of residual nickel In the filtrate(s) by atomic absorption spectrometry.
4.1.12.3 Document: ISO 4939:2016, Steel — Determination of nickel — Dimethyiglyoxime spectrophotometrk method.
Range of application:
— determination of nickel mass fractions in the range of 0,10% and 2,0% in steel. NOTE Cobalt, copper and manganese can cause Interferences, Principle of the method:
a) dissolution of a test portion in hydrochloric, nitric and perchlorlc acids;
b) lórmation of a coloured complex of nickel(lll) with dimethylglyoxime in ammoniacal solution containing iodine and potassium Iodide;
cJ spectrophotometric measurement at a wavelength olabout 535 nrn.
4.1.12.4 Document: ISO 13898-2:1997, Steel and iron — Determination of nickel, copper and cobalt contents — Inductively coupled plasma atomic emission speccrometric method — PUrl 2: Determination of nickel content.
Range of application:
— determination of nickel content between a mass traction of 0,001 % and a mass fraction of 0,30 % In unalloyed steel and unalloyed Iron.
Principle of the method:
a) dissolution of a test portion In a mixture of hydrochloric and nitric acids and dilution of the solution to known volume;
b) if necessary, addition of scandium or yttrium as rnternal standard;
C) nebulizatlon of the solution Into an ICP.AES and measurement of the Intensity of the emitted light from each element, or with emitted light from scandium or yttrium, simultaneously; examples of the analytical lines are given in ISO 13898.1:1997, Table 2.
4.1,13 NIobium, Nb
4.1.13.1 Document: ISO 9441:1988, Steel — Determination of niobium content — PAR specrrophotornetric method.
Range of application:
— determination of niobium content between a mass fraction of 0.005 % and a mass fraction of 1,3 % in steel.
Principle of the method:
a) dissolution of a test portion in hydrochloric acid followed by oxidation with hydrogen peroxide;
b) precipitation of niobium and tantalum with phenylarsonic acid, using zirconium as a carrier;
c) formation of a complex of niobium with 4(2-pyridyiazo)-resorcinol (PAR) in a sodium tartrate medium bulfered by sodium acetate solution adjusted to pH 6,3;
d) spectrophotometnc measurement of the coloured compound at a wavelength of about 500 nm.
4.1.13.2 Document: ISO 13899-2:2005, Steel — Determination of 140, Nb and W contents In aIhyed steel — Inductively coupled plasma atomic emission spectrometric method — Part 2: Determination of Nb content.
Range of application:
— determination of niobium content contents between a mass fraction oF 0.005 and a mass fraction of 5 % in steel.
Principle of the method:
a) the sample is dissolved in a hydrochloric, nitric and hydrofluoric acid mixture and fumed with a phosphoric and perchloric acid mixture; hydrofluoric acid and an Internal standard element (if used) are added and the solution Is diluted to known volume; the solution Is filtered and nebulized into an Inductively coupled plasma (ICP) and the intensity of the emitted light from each element is measured simultaneously with the light emitted from the internal standard element:
b) the method uses a calibration based on close matrix matching of the calibration solutions to the sample and close bracketing of the niobium content around the approximate concentration of niobium in the sample to be analysed; this compensates for matrix interferences and provides high accuracy, even in highly alloyed steels where spectral interferences can be severe; nonetheless, all interferences have to be kept to a minimum and iris therefore essential that the spectrometer used meets the performance criteria specified in the method for the selected analytical lines;
c) in order to accurately matrix match, it is necessary to know the concentration of all elements in the sample (to the nearest per cent); to this end, it may be necessary to carry out a preliminary analysis of the sample by some semi-quantitative method.
4.1.14 riltroge..N
4.1.14.1 Document: ISO 4945:2018, Steel — L)etermiriation of nitrogen — Spectrophotometric method. Range of application:
— dererminatmn of rntrogen mass fraction between 0,000 6 % and 0,050 % In low alloy steels and between 0,010% and 0,050% In high alloy steels.
N0Tl The method does not apply to samples containing silion nitrides or having sihcon contents higher than 0,6%.
Principle of the method:
a) dissolution ola test portion in dilute sulfuric acid:
bJ fuming of the acid-insoluble residue in sulfuric acid with potassium sulfate and copper(lI) sulfate;
C) distillation of the solution made alkaline with sodium hydroxide, and collection of ammonia In a receiver containing diluted sulfuric acid;
d) formation of a blue-coloured complex between the ammonlum ions and phenol in the presence of sodium hypochlorite and d isodium pentacyananitrosylferrate( Ill) (sodium nitroprusside);
e) spectrophotometric measurement of the complex at a wavelength of about 640 nm.
4.1.142 Document: ISO 10702:1993, Steel andiron — Determination of nitrogen content — Titrimetric
method after distillation.
Range of application:
— determination of nitrogen contents from a mass fraction of 0,002% toa mass fraction of 0,5% In steel and Iron;
— the method does not apply to samples containing silicon nitride.
Principle of the method:
a) dissolution ola test portion In hydrochloric acid followed by oxidation with hydrogen peroxide;
b) fuming of the acid-insoluble residue in sulfuric acid with potassium sulfate and copper(Il) sulfate:
c) distillation of the solution made alkaline with sodium hydroxide, and collection of ammonia in a receiver containing orthoboric acid solution;
d) titration of the ammonlum ion with amidosulfuric acid.
4.1.14.3 Document: ISO 10720:1997, Steel and iron — Determination of nitrogen content — Thermal
conductimetric method after fusion In a current of Inert gas.
Range of application:
— determination of nitrogen contents between a mass fraction of 0,000 8 % and a mass fraction of 0.5% in steel and Iron.
Principle of the method:
a) fusion of a test portion in a single-use graphite crucible under helium gas at a high temperature (e.g. 2 200 °C);
b) extraction of the nitrogen in the form of molecular nitrogen in the stream of helium:
c) separation from the other gaseous extracts and measurement by thermal conductimetrk method.
4.1.14.4 Document: ISO 15351:1999. Steel and iron — Determination of nitrogen content — Thermal conductimetric method after fusion in a current of inert gas (Routine method).
Range of application:
— determination of nitrogen contents between a mass fraction of 0,002 % and a mass fraction of 0.6 % in steel and Iron.
Principle of the method:
a) fusion of a test portion in a single-use graphite crucible under helium gas at a high temperature (e.g. 2 200 °C);
b) extraction of the nitrogen In the form of molecular nitrogen In the stream of helium:
c) separation from the other gaseous extracts and measurement by thermal conductimetric method:
d) calibration graph established using steel or iron certified reference materials (CRMs).
NOTE The accuracy of the tnethud Is largely dependent on the accuracy of the method used to certify the nitrogen concentration oICRMs as well as on their homogeneity. The calibration specimens used are ECRM, NIST, 1K, JSS. CMSI and other national or InternatIonal CRMs.
4.1.15 Oxygen,O
Document: ISO 17053:2005. Steel and iron — Determination 01 oxygen — Infrared method after fusion under inert gas.
Range of application:
— determination of mass fractions of oxygen between 0.000 75% and 0.01 % in steel and iron. Principle of the method:
a) fusion of a test portion In a single-use graphite crucible under helium gas at a minimum temperature of 2 000 ec; combination of the oxygen from the sample wIth carbon from the crucible to form carbon monoxide; eventually, transformation of carbon monoxide Into carbon dloxlde
b) measurement of infrared absorption of the carbon monoxide or dioxide, against a calibration curve made of potassium nitrate.
4.1.16 Phosphorus,P
Document: ISO 10714:1992. Steel and iron — Determination of phosphorus content — Pho.cpho vanadomolybd ate spectrophotometric method.
Range of application:
— determination of phosphorus contrnts between a mass fraction of 0,001 0% and a mass fraction of 1.0% In steel and iron.
NOTE Arsenic, hafnium, niobium, tantalum, titanium, and tungsten interfere in determining phosphorus. but the interferences can be partially overcome by formation of complexes and use of small quantities of test portion. Depending on the concentration of the interfering elements, the application ranges and test portions given in ISO 10714:1992. Table 1. apply.
Principle of the method:
a) dissolution of a test portion in an oxidizing acid mixture:
b) fuming with perchlorlc acid and removal of chromium as volatile chromyl chloride;
c) complexing of silicon and the refractory elements with hydrofluoric acid and complexing of the excess of bydrofluoric acid with orthoboric acid;
d) conversion of phosphorus to phusphovanado’molybdate in perchiork and nitric acid solution;
e) extraction of phosphovanadomolybdate by 4-methyl-2-pentanone with citric acid present to complex arsenic:
f) spectrophotometric measurement at a wavelength of 355 nm.
4.1.17 Sul(ur.S
4.1.17.1 Document: ISO 671:1982, Steel and cast fran — Determnat1on of sulphur content — Combustion titrimetric method.
Range of application:
— determination of sulfur in steel and cast iron, after combustion of the test portion in a current of oxygen.
Principle olthe method:
a) combustion of a test portion at a high temperature (1 450 °C) in a current of pure oxygen, if necessary in the presence ala metal flux:
b) transformation of sulfur into sulfur dioxide; absorption of the gases resulting from combustion. freed from oxide dust, by a solution of potassium sulfate and hydrogen peroxide;
c) titration of the absorbent solution with a standard sodium borate solution.
4.1.17.2 Document: ISO 4934:2003. Steel and iron — tktermination of sulfur content — Gravlmetrlc
mehod.
Range of application:
— determination of sulfur content between a mass fraction of 0.003 % and a mass fraction of 0,35 % in steels and iron, excluding steels containing selenium.
The method is particularly suitable as a reference method for the standardization of samples on which certified standard values are to be established.
Principle of the method:
a) dissolution of a test portion in dilute nitric acid in the presence of bromine, or in the mixed acid of nitric acid and hydrochloric acid in the presence of bromine (with the aid of an appropriate device to prevent sulfur losses):
b) additIon of perchloric acid and evaporation of the solution until white fumes of perchloric acid are evolved;
c) filtration of the solution and removal of the dehydrates of silicon. tungsten, niobium, etc;
d) addition of a determined quantity of sulfate ions to aid precipitation;
e) chromatographic separation of the sulfate ions from the test solution by adsorption on an alumina column, and elutlon using an ammonlum hydroxide solution;
f) precipitation of the sulfate ions as barium sulfate under controlled conditions and filtering. washing, heating and weighing.
4,1,17.3 Document: ISO 4935:1989, Steel and iron — Determmation of sulfur content — Infrared absorption method after combustion in an induction furnace.
Range of application:
— determination of sulfur content between a mass Fraction of 0,002% and a mass fraction of 0,10% In steel and Iron.
Principle of the method:
a) combustion of a test portion with accelerator at a high temperature in a high’frequency induction furnace In a current of pure oxygen; transformation of sulfur Into sulfur dioxide:
b) measurement by infrared absorption of the sulfur dioxide carried by a current of oxygen. 4.1.17.4 Document: ISO 10701:1994, Steel and irno — Determinutlon of sulfur content — Methylene blue
spectrophotometrlc method,
Range of application:
— determination of sulfur contents between a mass fraction of 0.000 3 % and a mass fraction of 0,010% in steel and iron.
NOTE Niobium, silicon, tantalum and titanium Interfere In the determination of sulfur. Depending on the concentranon of the Interfering elements, the application ranges and Lest portion masses given in ISO 10701:1994, Table 1. apply.
Principle of the method:
a) dissolution of a test portion In a mixture of hydrochloric and nitric acids;
b) evaporation with perchloric acid until white fumes appear to remove hydrochloric and nitric acids;
c) dissolution of the salts in hydrochloric acid; evolution of hydrogen sulfide by reducing with a mixture of hydroiodic and hypophosphorous acids in a nitrogen atmosphere, distillation, and absorption Into zinc acetate solution;
d) formation of methylene blue by reacting with N,N-dimethyl.p•phenylenediamine and lron(lll) solution;
e) spectrophotometric measurement at a wavelength of about 665 nm.
4.1.17.5 Document: 151) 13902:1997. Steel and iron — Determination of high sulfur content — Infrared absorption method after combustion in an inductfrn furnace.
Range of application:
— determination of sulfur content between a mass fraction of 0,10% and a mass tractIon of 0,35% in steel and Iron.
Principle of the method:
a) combustion of a test portion with accelerator at a high temperature in a high-frequency induction furnace in a current of pure oxygen:
b) transformation of sulfur Into sulfur dioxide:
c) measurement by Infrared absorption of the sulfur dioxide carried by a current of oxygen.
4.1.18 Siiicon,Sl
4.1.18.1 Document: ISO 439:1994, Steel and iron — Determination of total silicon content — Gravimetnc method.
Range of application:
— determination of the total silicon content between a mass fraction of 0,10% and a mass fraction of 5,0% In steel and Iron.
NOTE For samples containing molybdcnum, niobium, tantalum, titanium, tungsten, zirconium or high levels of chromium, the results are less pcecse than for unalloyed tterls,
Principle of the method:
a) attack ala test portion by hydrochloric and nitric acids;
b) conversion of acid-soluble silicon compounds to hydrated silicon dioxide by evaporation with perchloric acid until white fumes appear; filtration of the hydrated silicon dioxide and acid- insoluble silicon compounds, Ignition to form Impure silicon dioxide and then weighing;
c treatment of the Ignited residue with hydrofluoric and sulfuric acids, followed by Ignition and weighing.
4.1.18.2 Document: ISO 4829-1:2018, Steel and cast Iron — Determination of total silicon contents — Reduced molybdosilicate spectrophotometric method — Port 1: Silicon contents behveen 0,05 % and 1,0 %.
Range of application:
— determination of total silicon mass fraction between 0,05 % and 1,0 % in steel and cast iron. Principle of the method:
a) dissolution ola test portion in an acid mixture appropriatc to the alloy composition;
b) fusion of the acid-insoluble residue with sodium peroxide; formation olthe oxidized molybdosilicate (yellow) complex in weak acid solution:
c) selective reduction of the molybdosilicate complex to a blue complex with ascorbic acid, after Increasing the sulfuric acid concentration and adding axalic acid to prevent the interference of phosphorus, arsenic and vanadium;
d) spectrophatometric measurement of the reduced blue complex at a wavelength of about 810 nm.
4.1.18.3 Document: ISO 4829.2:2016, Steels — Determination of total silicon contents — Reduced molybdosrlicate spectmphotometrk method — Part 2: Silicon contents between 0.01 % and 0,05 %.
Range of application:
— determination of total silicon contents between a mass fraction of 0.01 % and a mass fraction of 0.05 % in steels.
Principle of the method:
a) dissolution ala test portion in a hydrochloric/nitric acids mixture;
b) fusion of the acid-insoluble residue with sodium peroxide; formation of the oxidized molybdosilicate (yellow) complex in weak acid solution:
c) selective reduction of the molybdosilicate complex to a blue complex with ascorbic acid, after increasing the sullurk acid concentration and adding oxalic acid to prevent the Interference of phosphorus, arsenic and vanadium;
d) spectrophotometric measurement of the reduced blue complex at a wavelength of about 810 nm.
4.1.18.4 Document: ISO/TR 17055:2002, Steel — Determination of silicon content — inductively coupled plasma atomic emission spectrometric method.
Range of application:
— determination of silicon content ala mass fraction 0,02% ba mass traction of S % in steel by means oIICP emission spectrometry.
Principle of the method:
a) the sample is dissolved in a hydrochloric, nitric and hydrofluoric acid mixture;
b) an internal standard element s added and the solution Is diluted to known volume;
c) the solution is nebulized into an ICP and the intensity of the emitted light from each clement Is measured simultaneously with the light emitted from the internal standard element.
4.1.19 Tln.Sn
Document: ISO 15353:2001. Steel and iron — Determination of tin content — Flame atomic absorption spectromethc method (extraction as Sn-SCN).
Range of application:
— determination of tin contents In the range 0,001 % by mass and 0,1 % by mass in steel and iron. Principle of the method:
a) dissolution of a test portion in hydrochloric and nitric acids: formation of Sn-SCN complex and extraction of the complex into 4-methyl-2-pentanone (isobutyl methyl ketone):
b) aspiration of the organic solution into a dinitrogen monoxide-acetylene flame; spectrometric measurement of the atomic absorption of the 224.6 nm spectral line emitted by a tin hollow cathode lamp;
c) high purity tin metal dissolved as standard solution is used as reference material for calibration graphs.
4.1.20 Titanium,Ti
Document: ISO 10280:1991, Steel and iron — Determination of titanium content — Dianttpyrylmethane spectrometric method.
Range olapplication:
— determination of titanium contents between a mass fraction of 0002 % and a mass fraction of 0.80% in steel and iron.
Principle of the method:
a) dissolution of a test portion in hydrochloric, nitric and sulfuric acids:
b) fusion of the residue with potassium hydrogen sulfate;
c) formation of a yellow complex with 4,4.diantipyryimcthane:
d) spectrophotometric measurement of the coloured complex at a wavelength of about 385 nm.
4.121 Tungsten.W
Document: ISO/TS 13899-3:2005, Steel — Determination of Mo. Nb and W contents in alloyed steel — Inductively coupled plasma atomic emission specrrometric method — Part 3: Determinat ion of W content
Range of application:
— determination of tungsten content between a mass fraction of 0,1 % and a mass fraction of 20 % in steel.
Principle of the method:
a) the sample is dissolved In a hydrochloric, nitric and hydrofluoric acid mixture and fumed with a phosphoric and perchioric acid mixture: hydrofluoric acid and an Internal standard element (II used) are added and the solution is diluted to known volume; the solution Is filtered and nebulized into an ICP spertrometer and the intensity of the emitted light from the element is measured simultaneously with the light emitted from the Internal standard element:
h) the method uses a calibration based on close matrix matching of the calibration solutions to the sample and close bracketing of the wngsten content around the approximate concentration of tungsten in the sample to be analysed; this compensates for matrix interferences and provides high accuracy, even In highly alloyed steels where spectral interferences can be severe; nonetheless, all Interferences have to be kept to a minimum and ft is therefore essential that the spectrometer used meets the performance criteria specified In the method for the selected analytical lines;
c) in order to accurately matrix match, it is necessary to know the content of all elements In the sample (to the nearest %); to this end. it may be necessary to carry out a preliminary analysis of the sample by a semi-quantitative method.
4.122 Vanadium.V
4.1.22.1 Document: ISO 4942:2016, Steels and Irons — Determination of vanadium content — N•BPHA spectrophotometrlc method.
Range of application:
— determination of vanadium contents between a mass fraction of 0,005 % and a mass fraction of 0.50% in steels and cast irons.
Principle of the method:
a) dissolution ola test portion with appropriate acids;
b) addition of orthophosphoric acid to an aliquot at the sample solution to prevent the interference of iron, and addition of potassium permanganate to oxidize vanadium to the pentavalent state;
c) selective reduction of excess permanganate by sodium nitrite, in the presence of urea and treatment with N-HPHA and hydrochloric acid to form a complex, followed by extraction of the complex with trlchloromethane;
d) spectrophotometric measurement of the absorbance at approximately 535 nm.
4122.2 Document: ISO 4947:1986. Steel und cast iron — Determination of vanadium content — Potentiometric titration method.
Range of application:
— determination of vanadium contents between a mass fraction of 0,04 % and a mass fraction of 2 % in steel and cast iron.
Principle of the method:
a) dissolution of a test portion with appropriate acids; addition of hydrofluoric acid to keep tungsten in solution;
b) oxidation of chromium and vanadium by potassium peroxy-disullate: partial oxidation of chromium;
c) while checking the potential of the solution:
— reduction oIchromium(Vl) and vanadium(V) by ammoclum iron(llJ sulfate;
— oxidation of vanadium by slight excess of potassium permanganate; reduction of the excess permangariate by sodium nitrite, and reduction of the excess sodium nitrite by sulfamic acid;
d) potentiometric titration of vanadium by ammonium iron(ll) sulfate standard solution.
4.122,3 Document: ISO 9647:1989, Steel and iron — Determination of vanadium content — Flame
atomic absorption spectrometric method.
Range of application:
— determination of vanadium contents between a mass fraction of 0.005 % and a mass fraction of 1.0 % In steel and iron, provided that the tungsten content in the test portion Is not higher than
10 mg and/or the titanium content Is not higher than S mg.
Principle of the method:
a) dissolution of a test portion In hydrochloric, nitric and perchlorlc acids;
b) addition olaluminlum solution as spectrochemical buffer;
c) spraying the solution into a dinitrogen monoxide-acetylene flame;
d) spectrometric measurement of the atomic absorption of the 318.4 nm spectral line emitted by a vanadium hollow cathode lamp.
4.2 Multi-elemental methods
4.2.1 Calcium, Ca; Magnesium. Mg
Document: ISO 13933:2014, Steel and iron — Determination of calcium and magnesium — Inductively coupled plasma atomic emission spectrometric method.
Range of application:
— determination of calcium content (mass fraction) In the range of 0,0005% to 0,006%;
— determination of magnesium contents (mass fraction) in the range of 0.000 5 % to 0,20 % in iron. cast iron, steel, and alloyed steeL
Principle of the method:
a) a test portion Is dissolved In a hydrochloric, nitric and hydrolluorlc acid mixture and fumed with perch loric acid;
b) hydrochloric acid, nitric acid, and an internal standard element (if used) are added and the solution Is diluted to a known volume;
c) the solution is Filtered, if necessary. nebulized into an ICP and the intensity of the emitted light from each element Is measured simultaneously with the intensity of the light emitted by the internal standard element.
4.2.2 Carbon, C; Sulfur, S
Document: ISO 15350:2000, Steel and iron — Determination of total carbon and sulfur content — Infrared absorption method after combustion in an Induction furnace (routine method).
Range of application:
— determination of carbon contents from a mass fraction of 0,005 % to a mass Iraction of 4,3 %;
— determination of sulfur contents from a mass fraction of 0.000 5 % to a mass fraction of 0,33 %.
Principle of the method.
a) the carbon Is converted to carbon monoxide and/or carbon dioxide by combustion In a stream of oxygen; measurement is by infrared absorption of the carbon monoxide and carbon dioxide carried by a current of oxygen:
b) the sulfur is converted to sulfur dioxide by combustion in a stream of oxygen: measurement is by infrared absorption of the sulfur dioxide carried by a current of oxygen.
4.2.3 Tin, Sn; Antimony, Sb; Cerium, Ce; Lead, Ph; Bismuth, 81
Document: ISO 16918-1:2009, Steel and iron — Determination of nine elements by the inductively coupled plasma mass spectrometric method — Part 1: DeterminatIon of tin, antimony, cerium, lead and bismuth.
Range of application:
— determination of tin contents from: 5 pg/g to 200 pg/g:
— determination of antimony contents from: 1 ig/g to 200 pg/g;
— determination of cerium contents from: 10 pg/g to 1 000 pg/g;
— determination of lead contents from: 0.5 agJg to 100 pgjg;
— determination of bismuth contents from: 0,3 pg/g to 30 i*g/g.
Principle of the method:
a) a test portion Is dissolved in an acid•mixture of hydrochloric acid, nitric acid and hydrofluoric acid using either a microwave.asslsted system or a traditional hot plate;
b) diluted wet-digested samples are introduced into an inductively coupled plasma mass spectrometer (ICP-MS), via a peristaltic pump: simultaneous measurements of the intensities of elements with atomic mass units of concern (mass spectra) are carried out using ICP-MS techniques;
c) calibration blank and calibration solutions are matrlx’matched with the major elements of steel, and mineral acids are used for wet•digestlon;
d) internal standards are used throughout in order to compensate for any instrument drilL
4.2.4 ChromIum, Cr Cobalt, Co; Copper. Cu; Manganese, Mn; Molybdenum, Mo: Nickel, NI; Niobium, Nb; Phosphorus. P; Silicon, Si; Titanium. TI; Vanadium, V
Document: ISO 17054:2010. Routine method fur analysis high a11oy steel by X-ray fluorescence spectrometry (XRF) by using a near•by technique.
Range of application:
— determination of chromium contents from a mass fraction of 10% to a mass traction of 25%;
— determination of cobalt contents from a mass fraction of 0,015 % to a mass fraction of 0,30 %;
— determination of copper contents from a mass fraction of 0,02% to mass fraction of 1.5%;
— determination of manganese contents from a mass fraction of 0,05 % to a mass fraction of 5.0%;
— determination of molybdenum contents from a mass fraction of 0.1 % to a mass fraction of 6,5 %;
— determination of nickel contents from a mass fraction of 0.1 % to a mass fraction of 30%;
— determination of niobium contents from a mass fraction of 0.05% to a mass fraction of 1.0%;
— determination of phosphorus contents from a mass fraction of 0,005% to a mass fraction of0.035%;
— determination of silicon contents from a mass fraction of 0.05% to a mass fraction of 1.5%;
— determination of titanium contents from a mass fraction of 0,015% to a mass fraction of 0,50%;
— determination of vanadium contents from a mass fraction of 0,015 % to a mass Fraction of 0,15 %.
The method is applicable to analysis of either chill-cast or wrought samples having a diameter of at
least 25 mm arid with a carbon concentration of less than 0.3 % (see NOTE). Other elements have a
concentration below 0.2 %.
NOTE High carbon concentrations. In comblnaflon with high Mo and Cr concentrations, could have undesirable structural effects on the sample and could affect the deierminaton o(phosphorus and chromium, in particular.
Principle of the method:
a) the sample Is finished to a clean uniform surface and then Irradiated by an X-ray beam olhlgh energy;
b) the secondary X-rays produced are dispersed by means of crystals and the intensities are measured by detectors at selected characteristic wavelengths; the measuring time is set to reach below a specified counting statistical error;
c) preliminary concentrations of the elements are determined by relatIng the measured intensities of unknown samples to analytical curves prepared from reference materials (CRMs or RMs) of known compositions; the final concentrations are calculated by using the results obtained by measuring a CRM of the same grade;
d) the correction is made for the elements ol interest by using the difference between the certified value and the value obtained during the measurement of the CRM (the ‘near-by technique’);
e) a fixed channel or a sequential system may be used to provide simultaneous or sequential determinations of element concentrations.
4.2.5 Zinc, Zn; Aluminium, Al; Nickel, NI; Iron, Fe; Silicon, Si; Lead. Pb
L)ocument: ISO 17925:2004, Zinc and/or aluminium based coatings on steel — Determination of coaling mass per unit area and chemical composition — Gravimetry. Inductively cou pled plasma atomic emission spectrometry and flame atomic absorption spectrometry.
Range of application:
— determination of zinc contents between a mass fraction of 40 % and a mass fraction of 100 %
— determination ol aluminium contents between a mass fraction ol 0.02% and a mass fraction o160 %;
— determination of nIckel contents between a mass fraction of 7 % and a mass fraction 0120%;
— determination of iron contents between a mass fraction of 0,2 % and a mass fraction of 20 %;
— determination of silicon contents between a mass traction of 0,2% and a mass fraction of 10%;
— determination of lead contents between a mass fraction of 0,005 % and a mass traction of 2 %.
NOTE 1 This method is applicable for the determination of the coating mass per unit area by gravimetry and the chemical composition of one side’surface or zinc and/or aluminium-based coatings on steel by means of ICP-AES or FAAS. For example, the test method applies for zinc and/or aluminium based coatings on steel such as galvanize (hot-dip and electrolytic) galvaneal (hot-dip), zinc-nickel electrolytic, zinc-5 % aluminium coating (hot.dip) and zinc.SS % aluminium coating (hot-dip). Galvanizing gives a pure zinc coating. Galvanealling gives a zinc-iron alloyed coating, Zinc-nickel electrolytic methods give zinc-nickel alloyed coatings.
NOTE For example, the applicable elements for these products are as follows: galvanizing is specified for iron and aluminium; galvanealling is specified for zinc, iron and aluminium; zinc•nickcd electrolytic methods are specified for zinc, Iron and nickel; zinc-S % aluminium coating Is specified for zinc, iron. aIuminum and silicon; zinc•SS % aluminium Is specified for zinc, Iron. aluminium and silicon.
Principle of the method:
a) stripping the coating on one side on the base steel in a mixture of hydrochloric acid solution containing an inhibitor to prevent the attack on the base steel; determination of the mass per unit area of coating from the mass difference of the specimen before and after stripping; calculating the coating mass as the mass difference divided by the specimen’s surface area;
b) dilution of the stripped solution of the coating on one side; filtration and nebulzatlon of the solution into an ICP’AES or flame atomic absorption spectrometer (FAAS): calculating the chemical compositions of coating layer as the content of the analytical element divided by the pre.measured coating mass.
42.6 Carbon, C; Silicon. SI; Manganese, Mn; Phosphorus, P; Sulfut S; Chromium. Cr Nickel, NI;
Aluminium, Al; Titanium, Ti; Copper, Cu:
Document: ISO 19272:2015, Low alloyed St eel — Determination of C, Si, Mn, P.S. Cr, Ni, Al, Ti and Cu – Glow
discharge optical emission spectrometry (routine method).
Range of application:
— determination of carbon contents from a mass fraction of 0,060% to a mass fraction of 0,35 %;
— determination of silicon contents from a mass fraction of 0,14 % to a mass fraction of 1,50 %;
— determination of manganese contents from a mass fraction of 0,090 % to a mass fraction of 0,70 %;
— determination of phosphorus contents from a mass fraction of 0.010 % to a mass fraction of 0,070 %;
— determination of sulfur contents from a mass fraction of 0,005 % to a mass fraction of 0,050 %;
— determination of chromium contents from a mass fraction of a mass fraction oF 0,008% to a mass fraction of 0,65 %;
— determination of nickel contents from a mass fraction of 0,050% to a mass fraction of 0.50%;
— determination of aluminium contents From a mass fraction of 0,006% to a mass fraction of 0,90 %;
— determination of titanium contents from a mass fraction of 0,014% to a mass fraction of 0,13%.
— determination of copper contents from a mass fraction o 0,005 % to a mass fraction of 1,00%.
Principle of the method:
a) a sample with a flat and smooth surface is used as the cathode of a direct current or radio frequency glow discharge device;
b) cathodic sputtering of the sample surface, diffusion of the sputtered atoms and ions from the sample surface; excitation of these awms and ions in the plasma formed in the glow discharge device;
c) spectrometric measurement of the intensity of the emitted light from the ions or the atoms of the elements to be determined, and, optionally, the emitted light from Iron at 371,994 nm or 271.441 nm or another appropriate wavelength (if Internal standard is used);
d) conversion of the measured signals to the contents through calibration curves established by measuring CRMs.
4.3 General documents
4.3.1 ThIs document, I.e. ISO/TR 9169;—. Steel and Iron — Review of available methods of analysis.
Scope: facilitates reference to published International Standards for the determination of the chemical composition of steel and iron.
4.3.2 Document: ISO 1389H1:1997, Steel and iron — Determination of nickeL copper and cobalt contents — Inductively coupled plasma atomic emission spectrometrlc method — Part 1: General requirements and sample dissolution.
Principle of the method:
a) specifies the general requirements for analysis by ICP-AES, preparation and dissolution of the Lest portion and method of calculation and the procedures used for the evaluation of the precision data of the individual methods specified in the subsequent parts;
b) specifies two alternative methods of evaluating concentrations in test solutions; one with and one without the use of an internal standard.
4.3.3 Document: ISO 14284:1996, Steel and Iron — Sampling and preparation of samples for the determination of chemical composition.
Principle of the method: specifies methods for sampling and sample preparation for the determination of the chemical composition of pig Iron. cast Iron and steel: methods are specifled for use with both liquid and solid metal.

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