Nickels, ferronickels and nickel alloys -- Standards for the determination of chemical composition

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.

Nickel, ferronickel et alliages de nickel -- Normes pour la détermination de la composition chimique

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Publication Date
26-Aug-2021
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5060 - Close of voting Proof returned by Secretariat
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TECHNICAL ISO/TR
REPORT 4644
First edition
2021-08
Nickels, ferronickels and nickel
alloys — Standards for the
determination of chemical
composition
Nickels, ferronickels et alliages de nickel — Normes pour la
détermination de la composition chimique
Reference number
ISO/TR 4644:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO/TR 4644:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/TR 4644:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 International Standards for the determination of the chemical composition of

nickels, ferronickels and nickel alloys ........................................................................................................................................... 2

4.1 Nickels ............................................................................................................................................................................................................ 2

4.2 Ferronickels ............................................................................................................................................................................................... 4

4.3 Nickel alloys ............................................................................................................................................................................................... 5

5 Range of application and principle of the methods ......................................................................................................... 6

5.1 Nickels ............................................................................................................................................................................................................ 6

5.1.1 Silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead and zinc

[Ag, Bi, Cd, Co, Cu, Fe, Mn, Pb and Zn] ............................................................................................................ 6

5.1.2 Silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin, tellurium

and thallium [Ag, As, Bi, Cd, Pb, Sb, Se, Sn, Te and Tl] ...................................................................... 7

5.1.3 Boron, B ................................................................................................................................................................................... 8

5.1.4 Phosphorus, P ..................................................................................................................................................................... 8

5.1.5 Sulfur, S ..................................................................................................................................................................................... 8

5.2 Ferronickels ............................................................................................................................................................................................... 9

5.2.1 Carbon, C ................................................................................................................................................................................. 9

5.2.2 Chromium, cobalt, copper, manganese and phosphorus [Cr, Co, Cu, Mn and P] ....... 9

5.2.3 Cobalt, Co .............................................................................................................................................................................10

5.2.4 Nickel, Ni ..............................................................................................................................................................................10

5.2.5 Phosphorus, P ..................................................................................................................................................................10

5.2.6 Sulfur, S ..................................................................................................................................................................................10

5.2.7 Silicon, Si ..............................................................................................................................................................................11

5.3 Nickel alloys ............................................................................................................................................................................................11

5.3.1 Aluminium, Al ..................................................................................................................................................................11

5.3.2 Boron, B ................................................................................................................................................................................12

5.3.3 Cobalt, chromium, copper, iron and manganese [Co, Cr, Cu, Fe and Mn] ......................12

5.3.4 Chromium, Cr ...................................................................................................................................................................12

5.3.5 Molybdenum, Mo ..........................................................................................................................................................12

5.3.6 Niobium, Nb ......................................................................................................................................................................13

5.3.7 Nickel, Ni ..............................................................................................................................................................................13

5.3.8 Phosphorus, P ..................................................................................................................................................................14

5.3.9 Lead, Pb .................................................................................................................................................................................14

5.3.10 Sulfur, S ..................................................................................................................................................................................15

5.3.11 Silicon, Si ..............................................................................................................................................................................15

5.3.12 Tantalum, Ta ...................................................................... ................................................................................................15

5.3.13 Titanium, Ti .......................................................................................................................................................................16

5.3.14 Vanadium, V ......................................................................................................................................................................16

Annex A (informative) Graphical representation of the scope of methods described in this

document ...................................................................................................................................................................................................................17

Annex B (informative) Bilingual key of the abbreviated terms used in the figures given in

Annex A ........................................................................................................................................................................................................................21

Bibliography .............................................................................................................................................................................................................................22

© ISO 2021 – All rights reserved iii
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ISO/TR 4644:2021(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO’s adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 155, Nickel and nickel alloys.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2021 – All rights reserved
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TECHNICAL REPORT ISO/TR 4644:2021(E)
Nickels, ferronickels and nickel alloys — Standards for the
determination of chemical composition
1 Scope

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.

2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
referee method

stoichiometric method or a method calibrated against pure metals or stoichiometric compounds, which

is used for certification analysis or in case of arbitration

Note 1 to entry: Due to a lack of accuracy or to a low number of laboratories having participated in the related

validation tests, some stoichiometric methods or methods calibrated against pure metals or stoichiometric

compounds cannot be taken as “referee methods”. They are published as Technical Specifications or Technical

Reports.
[SOURCE: CEN/TR 10261:2018, modified — Note 1 to entry has been added.]
3.2
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)

Note 1 to entry: By agreement, routine methods can be used for any commercial and/or arbitration purposes.

© ISO 2021 – All rights reserved 1
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ISO/TR 4644:2021(E)
[SOURCE: ISO/TR 9769:2018, modified — Note 1 to entry has been added.]
3.3
stoichiometry

founded on the “law of conservation of mass” where the total mass of the reactants equals the total mass

of the products, leading to the insight that the relations among quantities of reactants and products

typically form a ratio of positive integers
4 International Standards for the determination of the chemical composition of
nickels, ferronickels and nickel alloys
4.1 Nickels
4.1.1 Silver, Ag (referee methods)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.2 Arsenic, As (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.3 Boron, B (referee method)

ISO 11436:1993, Nickel and nickel alloys — Determination of total boron content — Curcumin molecular

absorption spectrometric method
4.1.4 Bismuth, Bi (referee methods)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.5 Cadmium, Cd (referee methods)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.6 Cobalt, Co (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
4.1.7 Copper, Cu (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
2 © ISO 2021 – All rights reserved
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ISO/TR 4644:2021(E)
4.1.8 Iron, Fe (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
4.1.9 Manganese, Mn (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
4.1.10 Phosphorus, P (referee method)

ISO 11400:1992, Nickel, ferronickel and nickel alloys — Determination of phosphorus content —

Phosphovanadomolybdate molecular absorption spectrometric method
4.1.11 Lead, Pb (referee methods)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.12 Antimony, Sb (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.13 Sulfur, S (referee method)

ISO 7527:1985, Nickel, ferronickel and nickel alloys — Determination of sulfur content — Iodimetric

titration method after induction furnace combustion
4.1.14 Selenium, Se (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.15 Tin, Sn (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.16 Tellurium, Te (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.17 Thallium, Tl (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.18 Zinc, Zn (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
© ISO 2021 – All rights reserved 3
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ISO/TR 4644:2021(E)
4.2 Ferronickels
4.2.1 Carbon, C (routine method)

ISO 7524:2020, Ferronickels — Determination of carbon content — Infrared absorption method after

induction furnace combustion
4.2.2 Chromium, Cr (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.3 Cobalt, Co (referee method)

ISO 7520:1985, Ferronickel — Determination of cobalt content — Flame atomic absorption spectrometric

method
4.2.4 Cobalt, Co (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.5 Copper, Cr (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.6 Manganese, Mn (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.7 Nickel, Ni (referee method)

ISO 6352:1985, Ferronickel — Determination of nickel content — Dimethylglyoxime gravimetric method

4.2.8 Phosphorus, P (referee method)

ISO 11400:1992, Nickel, ferronickel and nickel alloys — Determination of phosphorus content —

Phosphovanadomolybdate molecular absorption spectrometric method
4.2.9 Phosphorus, P (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.10 Sulfur, S (routine method)

ISO 7526:2020, Ferronickels — Determination of sulfur content — Infrared absorption method after

induction furnace combustion
4.2.11 Sulfur, S (referee method)

ISO 7527:1985, Nickel, ferronickel and nickel alloys — Determination of sulfur content — Iodimetric

titration method after induction furnace combustion
4 © ISO 2021 – All rights reserved
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ISO/TR 4644:2021(E)
4.2.12 Silicon, Si (referee method)

ISO 8343:1985, Ferronickel — Determination of silicon content — Gravimetric method

4.3 Nickel alloys
4.3.1 Aluminium, Al (referee method)

ISO 7530-7:1992, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 7: Determination

of aluminium content
4.3.2 Boron, B (referee method)

ISO 11436:1993, Nickel and nickel alloys — Determination of total boron content — Curcumin molecular

absorption spectrometric method
4.3.3 Cobalt, Co (referee method)

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.4 Chromium, Cr (referee methods)

ISO 7529:2017, Nickel alloys — Determination of chromium content — Potentiometric titration method

with ammonium iron(II) sulfate

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.5 Copper, Cu (referee method)

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.6 Iron, Fe (referee method)

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.7 Manganese, Mn (referee method)

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.8 Molybdenum, Mo (referee method)

ISO 11435:2011, Nickel alloys — Determination of molybdenum content — Inductively coupled plasma

atomic emission spectrometric method
4.3.9 Niobium, Nb (referee method)

ISO 22033:2011, Nickel alloys — Determination of niobium — Inductively coupled plasma atomic emission

spectrometric method
4.3.10 Nickel, Ni (referee method)

ISO/TS 18223:2015, Nickel alloys — Determination of Nickel content — Inductively coupled plasma atomic

emission spectrometric method
© ISO 2021 – All rights reserved 5
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ISO/TR 4644:2021(E)
4.3.11 Phosphorus, P (referee methods)

ISO 9388:1992, Nickel alloys — Determination of phosphorus content — Molybdenum blue molecular

absorption spectrometric method

ISO 11400:1992, Nickel, ferronickel and nickel alloys — Determination of phosphorus content —

Phosphovanadomolybdate molecular absorption spectrometric method
4.3.12 Lead, Pb (referee method)

ISO 11437:2018, Nickel alloys — Determination of lead — Electrothermal atomic absorption spectrometric

method
4.3.13 Sulfur, S (referee method)

ISO 7527:1985, Nickel, ferronickel and nickel alloys — Determination of sulfur content — Iodimetric

titration method after induction furnace combustion
4.3.14 Silicon, Si (referee method)

ISO 7530-8:1992, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 8: Determination

of silicon content
4.3.15 Tantalum, Ta (referee method)

ISO 23166:2018, Nickel alloys — Determination of tantalum — Inductively coupled plasma optical emission

spectrometric method
4.3.16 Titanium, Ti (referee method)

ISO 11433:2020, Nickel alloys — Determination of titanium content — Diantipyrylmethane molecular

absorption method
4.3.17 Vanadium, V (referee method)

ISO 7530-9:1993, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 9: Determination

of vanadium content
5 Range of application and principle of the methods
5.1 Nickels

5.1.1 Silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead and zinc [Ag, Bi, Cd, Co,

Cu, Fe, Mn, Pb and Zn]

Document: ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron,

manganese, lead and zinc contents — Flame atomic absorption spectrometric method.

Range of application:
— determination in refined, wrought and cast nickel of:
— silver contents from 0,000 2 % (by mass) to 0,01 % (by mass);
— bismuth contents from 0,001 0 % (by mass) to 0,01 % (by mass);
— cadmium contents from 0,000 2 % (by mass) to 0,002 5 % (by mass);
6 © ISO 2021 – All rights reserved
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ISO/TR 4644:2021(E)
— cobalt contents from 0,001 0 % (by mass) to 1,00 % (by mass);
— copper contents from 0,000 2 % (by mass) to 1,00 % (by mass);
— iron contents from 0,002 5 % (by mass) to 0,15 % (by mass);
— manganese contents from 0,000 5 % (by mass) to 0,20 % (by mass);
— lead contents from 0,000 5 % (by mass) to 0,01 % (by mass);
— zinc contents from 0,000 2 % (by mass) to 0,015 % (by mass).

NOTE 1 The upper limit for the determination of cobalt and copper can be raised to 2 % (by mass) by a minor

modification to the method.

NOTE 2 The lower limit for the determination of iron can be extended to less than 0,002 5 % (by mass)

provided nickel containing less than 0,000 1 % (by mass) iron is used for preparation of the standard solutions.

Principle of the method:

a) dissolution of a test portion in nitric acid diluted (1 + 1), evaporation of excess acid and dilution of

the solution to a known volume;

b) aspiration of the solution into the air-acetylene flame of an atomic absorption spectrometer;

c) measurement of the absorption of the resonance line energy from the spectrum of each element

and comparison with that of calibration solutions of the same element in a matched nickel matrix.

5.1.2 Silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin, tellurium and thallium

[Ag, As, Bi, Cd, Pb, Sb, Se, Sn, Te and Tl]

Document: ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony,

selenium, tin, tellurium and thallium contents — Electrothermal atomic absorption spectrometric method.

Range of application:
— determination in refined, wrought and cast nickel of:
— silver contents from 0,1 µg/g to 10 µg/g;
— arsenic contents from 1 µg/g to 20 µg/g;
— bismuth contents from 0,5 µg/g to 15 µg/g;
— cadmium contents from 0,1 µg/g to 2 µg/g;
— lead contents from 0,1 µg/g to 10 µg/g;
— antimony contents from 1 µg/g to 10 µg/g;
— selenium contents from 1 µg/g to 10 µg/g;
— tin contents from 1 µg/g to 5 µg/g;
— tellurium contents from 0,2 µg/g to 10 µg/g;
— thallium contents from 0,5 µg/g to 10 µg/g.
Principle of the method:

a) dissolution of a test portion in nitric acid 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;
© ISO 2021 – All rights reserved 7
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ISO/TR 4644:2021(E)

c) measurement of the absorption of the resonance line energy from the spectrum of each element

and comparison with that of calibration solutions of the same element in a matched nickel matrix

using background correction.
5.1.3 Boron, B

Document: ISO 11436:1993, Nickel and nickel alloys — Determination of total boron content — Curcumin

molecular absorption spectrometric method.
Range of application:

— determination of total boron contents from 4 µg/g to 240 µg/g in nickel and nickel alloys.

Principle of the method:
a) dissolution of a test portion in hydrochloric and nitric acids;

b) decomposition of resistant boron compounds (e.g. boron nitrides) by fuming the sample solution

with phosphoric and sulfuric acids at not less than 290 °C for 30 min;

c) formation of the boron curcumin complex in a buffered acetic acid and sulfuric acid medium;

d) measurement of the absorbance of the test solution at a wavelength of 543 nm.
5.1.4 Phosphorus, P

Document: ISO 11400:1992, Nickel, ferronickel and nickel alloys — Determination of phosphorus content

— Phosphovanadomolybdate molecular absorption spectrometric method.
Range of application:

— determination of phosphorus contents from 0,000 5 % (by mass) to 0,05 % (by mass) in nickel,

ferronickel and nickel alloys.

NOTE 1 As, Cr, Hf, Nb, Si, Ta, Ti, W interfere, but the interferences can be avoided by complexation or

volatilization (for Cr).

NOTE 2 The lowest phosphorus content (0,000 5 %) can only be reached in samples with low contents of the

interfering elements.
Principle of the method:
a) dissolution of a test portion in a mixture of nitric and hydrochloric acids;
b) fum
...

TECHNICAL ISO/TR
REPORT 4644
First edition
Nickel, ferronickel and nickel alloys —
Standards for the determination of
chemical composition
Nickel, ferronickel et alliages de nickel — Normes pour la
détermination de la composition chimique
PROOF/ÉPREUVE
Reference number
ISO/TR 4644:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO/TR 4644:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii PROOF/ÉPREUVE © ISO 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/TR 4644:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 International Standards for the determination of the chemical composition of

nickel, ferronickel and nickel alloys ................................................................................................................................................ 2

4.1 Nickel ............................................................................................................................................................................................................... 2

4.2 Ferronickel .................................................................................................................................................................................................. 4

4.3 Nickel alloys ............................................................................................................................................................................................... 5

5 Range of application and principle of the methods ......................................................................................................... 6

5.1 Nickel ............................................................................................................................................................................................................... 6

5.1.1 Silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead and zinc

[Ag, Bi, Cd, Co, Cu, Fe, Mn, Pb and Zn] ............................................................................................................ 6

5.1.2 Silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin, tellurium

and thallium [Ag, As, Bi, Cd, Pb, Sb, Se, Sn, Te and Tl] ...................................................................... 7

5.1.3 Boron, B ................................................................................................................................................................................... 8

5.1.4 Phosphorus, P ..................................................................................................................................................................... 8

5.1.5 Sulfur, S ..................................................................................................................................................................................... 8

5.2 Ferronickel .................................................................................................................................................................................................. 9

5.2.1 Carbon, C ................................................................................................................................................................................. 9

5.2.2 Chromium, cobalt, copper, manganese and phosphorus [Cr, Co, Cu, Mn and P] ....... 9

5.2.3 Cobalt, Co .............................................................................................................................................................................10

5.2.4 Nickel, Ni ..............................................................................................................................................................................10

5.2.5 Phosphorus, P ..................................................................................................................................................................10

5.2.6 Sulfur, S ..................................................................................................................................................................................10

5.2.7 Silicon, Si ..............................................................................................................................................................................11

5.3 Nickel alloys ............................................................................................................................................................................................11

5.3.1 Aluminium, Al ..................................................................................................................................................................11

5.3.2 Boron, B ................................................................................................................................................................................12

5.3.3 Cobalt, chromium, copper, iron and manganese [Co, Cr, Cu, Fe and Mn] ......................12

5.3.4 Chromium, Cr ...................................................................................................................................................................12

5.3.5 Molybdenum, Mo ..........................................................................................................................................................12

5.3.6 Niobium, Nb ......................................................................................................................................................................13

5.3.7 Nickel, Ni ..............................................................................................................................................................................13

5.3.8 Phosphorus, P ..................................................................................................................................................................14

5.3.9 Lead, Pb .................................................................................................................................................................................15

5.3.10 Sulfur, S ..................................................................................................................................................................................15

5.3.11 Silicon, Si ..............................................................................................................................................................................15

5.3.12 Tantalum, Ta ...................................................................... ................................................................................................15

5.3.13 Titanium, Ti .......................................................................................................................................................................16

5.3.14 Vanadium, V ......................................................................................................................................................................16

Annex A (informative) Graphical representation of the scope of methods described in this

document ...................................................................................................................................................................................................................17

Annex B (informative) Bilingual key of the abbreviated terms used in the figures given in

Annex A ........................................................................................................................................................................................................................21

Bibliography .............................................................................................................................................................................................................................22

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ISO/TR 4644:2021(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO’s adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 155, Nickel and nickel alloys.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv PROOF/ÉPREUVE © ISO 2021 – All rights reserved
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TECHNICAL REPORT ISO/TR 4644:2021(E)
Nickel, ferronickel and nickel alloys — Standards for the
determination of chemical composition
1 Scope

This document lists the International Standards which are currently available for the determination of

the chemical composition of nickel, ferronickel 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 nickel;
— Figure A.3 gives the content ranges of the methods for ferronickel;
— 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.

2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
referee method

stoichiometric method or a method calibrated against pure metals or stoichiometric compounds, which

is used for certification analysis or in case of arbitration

Note 1 to entry: Due to a lack of accuracy or to a low number of laboratories having participated in the related

validation tests, some stoichiometric methods or methods calibrated against pure metals or stoichiometric

compounds cannot be taken as “referee methods”. They are published as Technical Specifications or Technical

Reports.
[SOURCE: CEN/TR 10261:2018, modified — Note 1 to entry has been added.]
3.2
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)

Note 1 to entry: By agreement, routine methods can be used for any commercial and/or arbitration purposes.

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ISO/TR 4644:2021(E)
[SOURCE: ISO/TR 9769:2018, modified — Note 1 to entry has been added.]
3.3
stoichiometry

founded on the “law of conservation of mass” where the total mass of the reactants equals the total mass

of the products, leading to the insight that the relations among quantities of reactants and products

typically form a ratio of positive integers
4 International Standards for the determination of the chemical composition of
nickel, ferronickel and nickel alloys
4.1 Nickel
4.1.1 Silver, Ag (referee methods)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.2 Arsenic, As (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.3 Boron, B (referee method)

ISO 11436:1993, Nickel and nickel alloys — Determination of total boron content — Curcumin molecular

absorption spectrometric method
4.1.4 Bismuth, Bi (referee methods)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.5 Cadmium, Cd (referee methods)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.6 Cobalt, Co (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
4.1.7 Copper, Cu (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
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ISO/TR 4644:2021(E)
4.1.8 Iron, Fe (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
4.1.9 Manganese, Mn (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
4.1.10 Phosphorus, P (referee method)

ISO 11400:1992, Nickel, ferronickel and nickel alloys — Determination of phosphorus content —

Phosphovanadomolybdate molecular absorption spectrometric method
4.1.11 Lead, Pb (referee methods)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.12 Antimony, Sb (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.13 Sulfur, S (referee method)

ISO 7527:1985, Nickel, ferronickel and nickel alloys — Determination of sulfur content — Iodimetric

titration method after induction furnace combustion
4.1.14 Selenium, Se (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.15 Tin, Sn (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.16 Tellurium, Te (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.17 Thallium, Tl (referee method)

ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin,

tellurium and thallium contents — Electrothermal atomic absorption spectrometric method

4.1.18 Zinc, Zn (referee method)

ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead

and zinc contents — Flame atomic absorption spectrometric method
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ISO/TR 4644:2021(E)
4.2 Ferronickel
4.2.1 Carbon, C (routine method)

ISO 7524:2020, Ferronickels — Determination of carbon content — Infrared absorption method after

induction furnace combustion
4.2.2 Chromium, Cr (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.3 Cobalt, Co (referee method)

ISO 7520:1985, Ferronickel — Determination of cobalt content — Flame atomic absorption spectrometric

method
4.2.4 Cobalt, Co (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.5 Copper, Cr (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.6 Manganese, Mn (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.7 Nickel, Ni (referee method)

ISO 6352:1985, Ferronickel — Determination of nickel content — Dimethylglyoxime gravimetric method

4.2.8 Phosphorus, P (referee method)

ISO 11400:1992, Nickel, ferronickel and nickel alloys — Determination of phosphorus content —

Phosphovanadomolybdate molecular absorption spectrometric method
4.2.9 Phosphorus, Cr (referee method)

ISO 23156:2021, Ferronickels — Determination of phosphorus, manganese, chromium, copper and cobalt

contents — Inductively coupled plasma optical emission spectrometric method
4.2.10 Sulfur, S (routine method)

ISO 7526:2020, Ferronickels — Determination of sulfur content — Infrared absorption method after

induction furnace combustion
4.2.11 Sulfur, S (referee method)

ISO 7527:1985, Nickel, ferronickel and nickel alloys — Determination of sulfur content — Iodimetric

titration method after induction furnace combustion
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4.2.12 Silicon, Si (referee method)

ISO 8343:1985, Ferronickel — Determination of silicon content — Gravimetric method

4.3 Nickel alloys
4.3.1 Aluminium, Al (referee method)

ISO 7530-7:1992, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 7: Determination

of aluminium content
4.3.2 Boron, B (referee method)

ISO 11436:1993, Nickel and nickel alloys — Determination of total boron content — Curcumin molecular

absorption spectrometric method
4.3.3 Cobalt, Co (referee method)

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.4 Chromium, Cr (referee method)

ISO 7529:2017, Nickel alloys — Determination of chromium content — Potentiometric titration method

with ammonium iron(II) sulfate

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.5 Copper, Cu (referee method)

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.6 Iron, Fe (referee method)

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.7 Manganese, Mn (referee method)

ISO 7530-1:2015, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 1: Determination

of cobalt, chromium, copper, iron and manganese
4.3.8 Molybdenum, Mo (referee method)

ISO 11435:2011, Nickel alloys — Determination of molybdenum content — Inductively coupled plasma

atomic emission spectrometric method
4.3.9 Niobium, Nb (referee method)

ISO 22033:2011, Nickel alloys — Determination of niobium — Inductively coupled plasma atomic emission

spectrometric method
4.3.10 Nickel, Ni (referee method)

ISO/TS 18223:2015, Nickel alloys — Determination of Nickel content — Inductively coupled plasma atomic

emission spectrometric method
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ISO/TR 4644:2021(E)
4.3.11 Phosphorus, P (referee method)

ISO 9388:1992, Nickel alloys — Determination of phosphorus content — Molybdenum blue molecular

absorption spectrometric method

ISO 11400:1992, Nickel, ferronickel and nickel alloys — Determination of phosphorus content —

Phosphovanadomolybdate molecular absorption spectrometric method
4.3.12 Lead, Pb (referee method)

ISO 11437:2018, Nickel alloys — Determination of lead — Electrothermal atomic absorption spectrometric

method
4.3.13 Sulfur, S (referee method)

ISO 7527:1985, Nickel, ferronickel and nickel alloys — Determination of sulfur content — Iodimetric

titration method after induction furnace combustion
4.3.14 Silicon, Si (referee method)

ISO 7530-8:1992, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 8: Determination

of silicon content
4.3.15 Tantalum, Ta (referee method)

ISO 23166:2018, Nickel alloys — Determination of tantalum — Inductively coupled plasma optical emission

spectrometric method
4.3.16 Titanium, Ti (referee method)

ISO 11433:2020, Nickel alloys — Determination of titanium content — Diantipyrylmethane molecular

absorption method
4.3.17 Vanadium, V (referee method)

ISO 7530-9:1993, Nickel alloys — Flame atomic absorption spectrometric analysis — Part 9: Determination

of vanadium content
5 Range of application and principle of the methods
5.1 Nickel

5.1.1 Silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead and zinc [Ag, Bi, Cd, Co,

Cu, Fe, Mn, Pb and Zn]

Document: ISO 6351:1985, Nickel — Determination of silver, bismuth, cadmium, cobalt, copper, iron,

manganese, lead and zinc contents — Flame atomic absorption spectrometric method.

Range of application:
— determination in refined, wrought and cast nickel of:
— silver contents from 0,000 2 % (by mass) to 0,01 % (by mass);
— bismuth contents from 0,001 0 % (by mass) to 0,01 % (by mass);
— cadmium contents from 0,000 2 % (by mass) to 0,002 5 % (by mass);
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ISO/TR 4644:2021(E)
— cobalt contents from 0,001 0 % (by mass) to 1,00 % (by mass);
— copper contents from 0,000 2 % (by mass) to 1,00 % (by mass);
— iron contents from 0,002 5 % (by mass) to 0,15 % (by mass);
— manganese contents from 0,000 5 % (by mass) to 0,20 % (by mass);
— lead contents from 0,000 5 % (by mass) to 0,01 % (by mass);
— zinc contents from 0,000 2 % (by mass) to 0,015 % (by mass).

NOTE 1 The upper limit for the determination of cobalt and copper can be raised to 2 % (by mass) by a minor

modification to the method.

NOTE 2 The lower limit for the determination of iron can be extended to less than 0,002 5 % (by mass)

provided nickel containing less than 0,000 1 % iron is used for preparation of the standard solutions.

Principle of the method:

a) dissolution of a test portion in nitric acid diluted (1 + 1), evaporation of excess acid and dilution of

the solution to a known volume;

b) aspiration of the solution into the air-acetylene flame of an atomic absorption spectrometer;

c) measurement of the absorption of the resonance line energy from the spectrum of each element

and comparison with that of calibration solutions of the same element in a matched nickel matrix.

5.1.2 Silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin, tellurium and thallium

[Ag, As, Bi, Cd, Pb, Sb, Se, Sn, Te and Tl]

Document: ISO 7523:1985, Nickel — Determination of silver, arsenic, bismuth, cadmium, lead, antimony,

selenium, tin, tellurium and thallium contents — Electrothermal atomic absorption spectrometric method.

Range of application:
— determination in refined, wrought and cast nickel of:
— silver contents from 0,1 µg/g (by mass) to 10 µg/g (by mass);
— arsenic contents from 1 µg/g (by mass) to 20 µg/g (by mass);
— bismuth contents from 0,5 µg/g (by mass) to 15 µg/g (by mass);
— cadmium contents from 0,1 µg/g (by mass) to 2 µg/g (by mass);
— lead contents from 0,1 µg/g (by mass) to 10 µg/g (by mass);
— antimony contents from 1 µg/g (by mass) to 10 µg/g (by mass);
— selenium contents from 1 µg/g (by mass) to 10 µg/g (by mass);
— tin contents from 1 µg/g (by mass) to 5 µg/g (by mass);
— tellurium contents from 0,2 µg/g (by mass) to 10 µg/g (by mass);
— thallium contents from 0,5 µg/g (by mass) to 10 µg/g (by mass).
Principle of the method:

a) dissolution of a test portion in nitric acid 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;
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c) measurement of the absorption of the resonance line energy from the spectrum of each element

and comparison with that of calibration solutions of the same element in a matched nickel matrix

using background correction.
5.1.3 Boron, B

Document: ISO 11436:1993, Nickel and nickel alloys — Determination of total boron content — Curcumin

molecular absorption spectrometric method.
Range of application:

— determination of total boron contents from 4 µg/g (by mass) to 240 µg/g (by mass) in nickel and

nickel alloys.
Principle of the method:
a) dissolution of a test portion in hydrochloric and nitric acids;

b) decomposition of resistant boron compounds (e.g. boron nitrides) by fuming the sample solution

with phosphoric and sulfuric acids at not less than 290 °C for 30 min;

c) formation of the boron curcumin complex in a buffered acetic acid and sulfuric acid medium;

d) measurement of the absorbance of the test solution at a wavelength of 543 nm.
5.1.4 Phosphorus, P

Document: ISO 11400:1992, Nickel, ferronickel and nickel alloys — Determination of phosphorus content

— Phosphovanadomolybdate molecular absorption spectrometric method.
Range of application:

— determination of phosphorus contents from 0,000 5 % (by mass) to 0,05 % (by mass) in nickel,

ferronickel and nickel alloys.
NOTE 1 As, Cr, Hf, Nb, Si, T
...

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