Ferronickels -- Determination of phosphorus, manganese, chromium, copper and cobalt contents -- Inductively coupled plasma optical emission spectrometric method

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

Ferro-nickels -- Détermination du phosphore, du manganèse, du chrome, du cuivre et du cobalt -- Méthode par spectrométrie d'émission optique avec plasma induit par haute fréquence

General Information

Status
Published
Publication Date
25-Mar-2021
Current Stage
5060 - Close of voting Proof returned by Secretariat
Start Date
17-Feb-2021
Completion Date
17-Feb-2021
Ref Project

Buy Standard

Standard
ISO 23156:2021 - Ferronickels -- Determination of phosphorus, manganese, chromium, copper and cobalt contents -- Inductively coupled plasma optical emission spectrometric method
English language
16 pages
sale 15% off
Preview
sale 15% off
Preview
Draft
ISO/PRF 23156:Version 30-jan-2021 - Ferronickels -- Determination of phosphorus, manganese, chromium, copper and cobalt contents -- Inductively coupled plasma optical emission spectrometric method
English language
15 pages
sale 15% off
Preview
sale 15% off
Preview

Standards Content (sample)

INTERNATIONAL ISO
STANDARD 23156
First edition
2021-03
Ferronickels — Determination of
phosphorus, manganese, chromium,
copper and cobalt contents —
Inductively coupled plasma optical
emission spectrometric method
Ferro-nickels — Détermination du phosphore, du manganèse,
du chrome, du cuivre et du cobalt — Méthode par spectrométrie
d'émission optique avec plasma induit par haute fréquence
Reference number
ISO 23156:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 23156:2021(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 23156:2021(E)
Contents Page

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

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

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

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

4 Principle ........................................................................................................................................................................................................................ 2

5 Reagents ........................................................................................................................................................................................................................ 2

6 Apparatus ..................................................................................................................................................................................................................... 4

6.1 General ........................................................................................................................................................................................................... 4

6.2 Instrument performance requirements ............................................................................................................................ 4

6.2.1 Wavelengths ......................................................................................................................................................................... 4

6.2.2 Practical resolution of the spectrometer .................................................................................................... 5

6.2.3 Short-term stability ....................................................................................................................................................... 5

6.2.4 Background equivalent concentration .......................................................................................................... 5

6.2.5 Linearity of the calibration curves ................................................................................................................... 5

7 Sampling and sample preparation .................................................................................................................................................... 5

8 Procedure..................................................................................................................................................................................................................... 5

8.1 Test portion ................................................................................................................................................................................................ 5

8.2 Preparation of the test solution ................................................................................................................................................ 6

8.3 Preparation of the calibration solutions ........................................................................................................................... 6

8.4 Optimization of the instrument ................................................................................................................................................ 7

8.5 Measurements ......................................................................................................................................................................................... 7

8.5.1 Measurement of the calibration solutions ................................................................................................. 7

8.5.2 Measurement of the test solutions ................................................................................................................... 8

8.6 Calibration curves ................................................................................................................................................................................ 8

9 Expression of the results .............................................................................................................................................................................. 8

9.1 Calculation of results ......................................................................................................................................................................... 8

9.2 Precision ....................................................................................................................................................................................................... 8

9.2.1 Interlaboratory test ....................................................................................................................................................... 8

9.2.2 Precision data ..................................................................................................................................................................... 8

9.3 Trueness ....................................................................................................................................................................................................10

10 Test report ................................................................................................................................................................................................................12

Annex A (normative) Checking the performance of an inductively coupled plasma optical

emission spectrometer ...............................................................................................................................................................................13

Annex B (informative) Notes on the interlaboratory test ............................................................................................................15

Bibliography .............................................................................................................................................................................................................................16

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 23156:2021(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
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 23156:2021(E)
Ferronickels — Determination of phosphorus, manganese,
chromium, copper and cobalt contents — Inductively
coupled plasma optical emission spectrometric method
1 Scope

This document specifies a method for the determination of phosphorus, manganese, chromium, copper

and cobalt contents in ferronickels, by inductively coupled plasma (ICP) optical emission spectrometry,

within the ranges specified in Table 1.
This method is applicable to all grades of ferronickels specified in ISO 6501.
Table 1 — Application ranges of the elements to be determined
Application range
Element
% (mass fraction)
Phosphorus 0,009 to 0,045
Manganese 0,02 to 1,0
Chromium 0,076 to 1,86
Cobalt 0,24 to 1,4
Copper 0,02 to 0,07
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 385, Laboratory glassware — Burettes
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 8049, Ferronickel shot — Sampling for analysis
ISO 8050, Ferronickel ingots or pieces — Sampling for analysis
3 Terms and definitions
No terms and definitions are listed in this document.

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/
© ISO 2021 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 23156:2021(E)
4 Principle

Dissolution of a test portion with nitric, hydrochloric and hydrofluoric acids. Addition of perchloric

acid to remove fluorine and silicon. Addition of nitric and hydrochloric acids to dissolve the salts. After

suitable dilution and, if necessary, addition of an internal reference element, nebulization of the solution

into an ICP optical emission spectrometer and measurement of the intensity of the emitted light from

each element (including, where relevant, the intensity of the internal reference element).

5 Reagents

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only

Grade 2 water as specified in ISO 3696.

The same reagents should be used for the preparation of calibration solutions and of sample solutions.

5.1 Pure nickel, containing less than 0,001 % (mass fraction) of P, Mn, Cr, Cu and Co.

5.2 Pure iron, containing less than 0,001 % (mass fraction) of P, Mn, Cr, Cu and Co.

5.3 Hydrochloric acid, HCl, ρ = 1,19 g/ml.
5.4 Nitric acid, HNO , ρ = 1,40 g/ml.
3 20
5.5 Nitric acid, HNO , diluted 1 + 1.
Add 500 ml of nitric acid (5.4) to 500 ml of water and mix.
5.6 Hydrofluoric acid, HF, ρ = 1,14 g/ml.

WARNING — Hydrofluoric acid is extremely irritating and corrosive to skin and mucous

membranes producing severe skin burns which are slow to heal. In case of contact with skin,

wash well with water, apply a topical gel containing 2,5 % (mass fraction) calcium gluconate and

seek immediate medical treatment.
5.7 Perchloric acid, HClO , ρ = 1,54 g/ml.
4 20

WARNING — Perchloric acid vapour may cause explosion in the presence of ammonia, nitrous

fume or organic matter in general. All evaporation shall be carried out in fume hood specifically

designed for the use of perchloric acid.
5.8 Sulfuric acid, H SO , ρ = 1,84 g/ml.
2 4 20
5.9 Internal reference element solution, 1 g/l.

Weigh (1,27 ± 0,001) g of yttrium oxide [minimum purity 99,98 % (mass fraction)] and dissolve in 50 ml

of hydrochloric acid (5.3). Transfer the solution quantitatively into a 1 000 ml one-mark volumetric

flask, dilute to the mark with water and mix.
1 ml of this internal reference element solution contains 1 mg of yttrium.
NOTE Commercially available standard solutions are also used for this purpose.
5.10 Internal reference element solution, 10 mg/l.

Transfer 10,0 ml of the internal reference element solution (5.9) into a 1 000 ml one-mark volumetric

flask, add 50 ml of hydrochloric acid (5.3), dilute to the volume with water and mix.

2 © ISO 2021 – All rights reserved
---------------------- Page: 6 ----------------------
ISO 23156:2021(E)
1 ml of this internal reference element solution contains 10 µg of yttrium.
5.11 Phosphorus standard solution, 1 g/l.

Weigh (2,197 ± 0,001) g of potassium dihydrogen phosphate, previously dried to constant mass at 110 °C

and cooled in a desiccator. Dissolve it in a 250 ml beaker with water. Transfer the solution quantitatively

into a 500 ml one-mark volumetric flask, dilute to the volume with water and mix.

1 ml of this solution contains 1 mg of phosphorus.
5.12 Phosphorus standard solution, 0,25 g/l.

Transfer 25,0 ml of the phosphorus standard solution (5.11) into a 100 ml one-mark volumetric flask,

dilute to the volume with water and mix.
1 ml of this standard solution contains 0,25 mg of phosphorus.
5.13 Manganese standard solution, 1 g/l.

The manganese used to prepare the solution is released from superficial oxide possibly present by

introducing a few grams of metal in a 250 ml beaker containing 150 ml to 160 ml of water and 15 ml to

20 ml of sulphuric acid (5.8). Shake and after a few seconds, allow the solution to settle and add water.

Repeat the water cleaning several times. Remove the metallic manganese and rinse with acetone. Dry

the metal in an oven at 100 °C for 2 min or with a hairdryer. Cool in a desiccator.

Weigh (0,5 ± 0,001) g of manganese [minimum purity 99,95 % (mass fraction)] and transfer into a

250 ml beaker. Add 5 ml of hydrochloric acid (5.3) and 10 ml of nitric acid (5.5). Cover with a watch-

glass and heat gently until the metal is dissolved. Boil to remove nitrogen oxides. After cooling, transfer

the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the volume with water

and mix.
1 ml of this solution contains 1 mg of manganese.
5.14 Chromium standard solution, 1 g/l.

Weigh (0,5 ± 0,001) g of chromium [minimum purity 99,99 % (mass fraction)] and transfer into a 250 ml

beaker. Add 40 ml of hydrochloric acid (5.3), cover with a watch-glass and heat gently until the metal

is completely dissolved. After cooling, transfer the solution quantitatively into a 500 ml one-mark

volumetric flask, dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of chromium.
5.15 Copper standard solution, 1 g/l.

Weigh (0,5 ± 0,001) g of copper [minimum purity 99,95 % (mass fraction)] and transfer into a 250 ml

beaker. Add 30 ml of nitric acid (5.5), cover with a watch-glass and heat gently until the metal is

dissolved. Boil to remove nitrogen oxides. After cooling, transfer the solution quantitatively into a

500 ml one-mark volumetric flask, dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of copper.
5.16 Cobalt standard solution, 1 g/l.

Weigh (0,5 ± 0,001) g of cobalt [minimum purity 99,95 % (mass fraction)] and transfer into a 250 ml

beaker. Add 40 ml of nitric acid (5.5), cover with a watch-glass and heat gently until the metal is

dissolved. Boil to remove nitrogen oxides. After cooling, transfer the solution quantitatively into a

500 ml one-mark volumetric flask, dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of cobalt.
© ISO 2021 – All rights reserved 3
---------------------- Page: 7 ----------------------
ISO 23156:2021(E)
5.17 Cobalt standard solution, 0,25 g/l.

Transfer 25,0 ml of the cobalt standard solution (5.16) into a 100 ml one-mark volumetric flask, dilute

to the volume with water and mix.
1 ml of this standard solution contains 0,25 mg of cobalt.
5.18 Multi-elemental standard solution of copper and phosphorus

Transfer 5,0 ml of the copper standard solution (5.15) and 10,0 ml of the phosphorus standard solution

(5.12) into a 100 ml one-mark volumetric flask, dilute to the volume with 5 ml of nitric acid (5.5) and

water then mix.

1 ml of this standard solution respectively contains 50 µg of copper and 25 µg of phosphorus.

5.19 Multi-elemental standard solution of manganese and chromium

Transfer 10,0 ml of the manganese standard solution (5.13) and 25,0 ml of the chromium standard

solution (5.14) into a 100 ml one-mark volumetric flask, dilute to the volume with water and mix.

1 ml of this standard solution respectively contains 0,10 mg of manganese and 0,25 mg of chromium.

6 Apparatus
6.1 General
Ordinary laboratory apparatus and the following.

All volumetric glassware shall be class A and calibrated in accordance with ISO 385, ISO 648 or

ISO 1042, as appropriate.
6.1.1 Polytetrafluoroethylene (PTFE) beakers, of capacity 250 ml.
6.1.2 Polypropylene volumetric flasks, of capacity 100 ml.
6.1.3 Optical emission spectrometer (OES), equipped with ICP.

The spectrometer shall be equipped with a nebulization system. The instrument used will be

satisfactory if, after optimizing in accordance with the manufacturer’s instructions, it meets the

performance requirements given in 6.2.1 to 6.2.5.

The spectrometer can be either a simultaneous or a sequential one. If a sequential spectrometer can be

equipped with an extra arrangement for simultaneous measurement of the internal reference element

line, it can be used with the internal reference element method. If the sequential spectrometer is not

equipped with this arrangement, an internal reference element cannot be used and an alternative

method without an internal reference element should be applied.
6.2 Instrument performance requirements
6.2.1 Wavelengths
This document does not specify particular wavelengths. It is mandatory that
...

INTERNATIONAL ISO
STANDARD 23156
First edition
Ferronickels – Determination of
phosphorus, manganese, chromium,
copper and cobalt contents –
Inductively coupled plasma optical
emission spectrometric method
PROOF/ÉPREUVE
Reference number
ISO 23156:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 23156:2021(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 23156:2021(E)
Contents Page

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

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

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

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

4 Principle ........................................................................................................................................................................................................................ 2

5 Reagents ........................................................................................................................................................................................................................ 2

6 Apparatus ..................................................................................................................................................................................................................... 4

6.1 General ........................................................................................................................................................................................................... 4

6.2 Instrument performance requirements ............................................................................................................................ 4

6.2.1 Wavelengths ......................................................................................................................................................................... 4

6.2.2 Practical resolution of the spectrometer .................................................................................................... 5

6.2.3 Short-term stability ....................................................................................................................................................... 5

6.2.4 Background equivalent concentration .......................................................................................................... 5

6.2.5 Linearity of the calibration curves ................................................................................................................... 5

7 Sampling and sample preparation .................................................................................................................................................... 5

8 Procedure..................................................................................................................................................................................................................... 5

8.1 Test portion ................................................................................................................................................................................................ 5

8.2 Preparation of the test solution ................................................................................................................................................ 6

8.3 Preparation of the calibration solutions ........................................................................................................................... 6

8.4 Optimization of the instrument ................................................................................................................................................ 7

8.5 Measurements ......................................................................................................................................................................................... 7

8.5.1 Measurement of the calibration solutions ................................................................................................. 7

8.5.2 Measurement of the test solutions ................................................................................................................... 8

8.6 Calibration curves ................................................................................................................................................................................ 8

9 Expression of the results .............................................................................................................................................................................. 8

9.1 Calculation of results ......................................................................................................................................................................... 8

9.2 Precision ....................................................................................................................................................................................................... 8

9.2.1 Interlaboratory test ....................................................................................................................................................... 8

9.2.2 Precision data ..................................................................................................................................................................... 8

9.3 Trueness ....................................................................................................................................................................................................... 9

10 Test report ................................................................................................................................................................................................................11

Annex A (normative) Checking the performance of an inductively coupled plasma optical

emission spectrometer ...............................................................................................................................................................................12

Annex B (informative) Notes on the interlaboratory test ............................................................................................................14

Bibliography .............................................................................................................................................................................................................................15

© ISO 2021 – All rights reserved PROOF/ÉPREUVE iii
---------------------- Page: 3 ----------------------
ISO 23156:2021(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
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 23156:2021(E)
Ferronickels – Determination of phosphorus, manganese,
chromium, copper and cobalt contents – Inductively
coupled plasma optical emission spectrometric method
1 Scope

This document specifies a method for the determination of phosphorus, manganese, chromium, copper

and cobalt contents in ferronickels, by inductively coupled plasma (ICP) optical emission spectrometry,

within the ranges specified in Table 1.
This method is applicable to all grades of ferronickels specified in ISO 6501.
Table 1 — Application ranges of the elements to be determined
Application range
Element
% (mass fraction)
Phosphorus 0,009 to 0,045
Manganese 0,02 to 1,0
Chromium 0,076 to 1,86
Cobalt 0,24 to 1,4
Copper 0,02 to 0,07
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 385, Laboratory glassware — Burettes
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 8049, Ferronickel shot — Sampling for analysis
ISO 8050, Ferronickel ingots or pieces — Sampling for analysis
3 Terms and definitions
No terms and definitions are listed in this document.

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/
© ISO 2021 – All rights reserved PROOF/ÉPREUVE 1
---------------------- Page: 5 ----------------------
ISO 23156:2021(E)
4 Principle

Dissolution of a test portion with nitric, hydrochloric and hydrofluoric acids. Addition of perchloric

acid to remove fluorine and silicon. Addition of nitric and hydrochloric acids to dissolve the salts. After

suitable dilution and, if necessary, addition of an internal reference element, nebulization of the solution

into an ICP optical emission spectrometer and measurement of the intensity of the emitted light from

each element (including, where relevant, the intensity of the internal reference element).

5 Reagents

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only

Grade 2 water as specified in ISO 3696.

The same reagents should be used for the preparation of calibration solutions and of sample solutions.

5.1 Pure nickel, containing less than 0,001 % (mass fraction) of P, Mn, Cr, Cu and Co.

5.2 Pure iron, containing less than 0,001 % (mass fraction) of P, Mn, Cr, Cu and Co.

5.3 Hydrochloric acid, HCl, ρ = 1,19 g/ml.
5.4 Nitric acid, HNO , ρ = 1,40 g/ml.
3 20
5.5 Nitric acid, HNO , diluted 1 + 1.
Add 500 ml of nitric acid (5.4) to 500 ml of water and mix.
5.6 Hydrofluoric acid, HF, ρ = 1,14 g/ml.

WARNING — Hydrofluoric acid is extremely irritating and corrosive to skin and mucous

membranes producing severe skin burns which are slow to heal. In case of contact with skin,

wash well with water, apply a topical gel containing 2,5 % (mass fraction) calcium gluconate and

seek immediate medical treatment.
5.7 Perchloric acid, HClO , ρ = 1,54 g/ml.
4 20

WARNING — Perchloric acid vapour may cause explosion in the presence of ammonia, nitrous

fume or organic matter in general. All evaporation shall be carried out in fume hood specifically

designed for the use of perchloric acid.
5.8 Sulfuric acid, H SO , ρ = 1,84 g/ml.
2 4 20
5.9 Internal reference element solution, 1 g/l.

Weigh (1,27 ± 0,001) g of yttrium oxide [minimum purity 99,98 % (mass fraction)] and dissolve in 50 ml

of hydrochloric acid (5.3). Transfer the solution quantitatively into a 1 000 ml one-mark volumetric

flask, dilute to the mark with water and mix.
1 ml of this internal reference element solution contains 1 mg of yttrium.
NOTE Commercially available standard solutions are also used for this purpose.
5.10 Internal reference element solution, 10 mg/l.

Transfer 10,0 ml of the internal reference element solution (5.9) into a 1 000 ml one-mark volumetric

flask, add 50 ml of hydrochloric acid (5.3), dilute to the volume with water and mix.

2 PROOF/ÉPREUVE © ISO 2021 – All rights reserved
---------------------- Page: 6 ----------------------
ISO 23156:2021(E)
1 ml of this internal reference element solution contains 10 µg of yttrium.
5.11 Phosphorus standard solution, 1 g/l.

Weigh (2,197 ± 0,001) g of potassium dihydrogen phosphate, previously dried to constant mass at 110 °C

and cooled in a desiccator. Dissolve it in a 250 ml beaker with water. Transfer the solution quantitatively

into a 500 ml one-mark volumetric flask, dilute to the volume with water and mix.

1 ml of this solution contains 1 mg of phosphorus.
5.12 Phosphorus standard solution, 0,25 g/l.

Transfer 25 ml of the phosphorus standard solution (5.11) into a 100 ml one-mark volumetric flask,

dilute to the volume with water and mix.
1 ml of this standard solution contains 0,25 mg of phosphorus.
5.13 Manganese standard solution, 1 g/l.

The manganese used to prepare the solution is released from superficial oxide possibly present by

introducing a few grams of metal in a 250 ml beaker containing 150 ml to 160 ml of water and 15 ml to

20 ml of sulphuric acid (5.8). Shake and after a few seconds, allow the solution to settle and add water.

Repeat the water cleaning several times. Remove the metallic manganese and rinse with acetone. Dry

the metal in an oven at 100 °C for 2 min or with a hairdryer. Cool in a desiccator.

Weigh (0,5 ± 0,001) g of manganese [minimum purity 99,95 % (mass fraction)] and transfer into a

250 ml beaker. Add 5 ml of hydrochloric acid (5.3) and 10 ml of nitric acid solution (5.5). Cover with a

watch-glass and heat gently until the metal is dissolved. Boil to remove nitrogen oxides. After cooling,

transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the volume with

water and mix.
1 ml of this solution contains 1 mg of manganese.
5.14 Chromium standard solution, 1 g/l.

Weigh (0,5 ± 0,001) g of chromium [minimum purity 99,99 % (mass fraction)] and transfer into a 250 ml

beaker. Add 40 ml of hydrochloric acid (5.3), cover with a watch-glass and heat gently until the metal

is completely dissolved. After cooling, transfer the solution quantitatively into a 500 ml one-mark

volumetric flask, dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of chromium.
5.15 Copper standard solution, 1 g/l.

Weigh (0,5 ± 0,001) g of copper [minimum purity 99,95 % (mass fraction)] and transfer into a 250 ml

beaker. Add 30 ml of nitric acid solution (5.5), cover with a watch-glass and heat gently until the metal

is dissolved. Boil to remove nitrogen oxides. After cooling, transfer the solution quantitatively into a

500 ml one-mark volumetric flask, dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of copper.
5.16 Cobalt standard solution, 1 g/l.

Weigh (0,5 ± 0,001) g of cobalt [minimum purity 99,95 % (mass fraction)] and transfer into a 250 ml

beaker. Add 40 ml of nitric acid solution (5.5), cover with a watch-glass and heat gently until the metal

is dissolved. Boil to remove nitrogen oxides. After cooling, transfer the solution quantitatively into a

500 ml one-mark volumetric flask, dilute to the volume with water and mix.
1 ml of this solution contains 1 mg of cobalt.
© ISO 2021 – All rights reserved PROOF/ÉPREUVE 3
---------------------- Page: 7 ----------------------
ISO 23156:2021(E)
5.17 Cobalt standard solution, 0,25 g/l.

Transfer 25,0 ml of the cobalt standard solution (5.16) into a 100 ml one-mark volumetric flask, dilute

to the volume with water and mix.
1 ml of this standard solution contains 0,250 mg of cobalt.
5.18 Multi-elemental standard solution of copper and phosphorus

Transfer 5,0 ml of the copper standard solution (5.15) and 10,0 ml of the phosphorus standard solution

(5.12) into a 100 ml one-mark volumetric flask, dilute to the volume with nitric acid solution (5.5) and mix.

1 ml of this standard solution respectively contains 50 µg of copper and 25 µg of phosphorus.

5.19 Multi-elemental standard solution of manganese and chromium

Transfer 10,0 ml of the manganese standard solution (5.13) and 25,0 ml of the chromium standard

solution (5.14) into a 100 ml one-mark volumetric flask, dilute to the volume with water and mix.

1 ml of this standard solution respectively contains 0,10 mg of manganese and 0,25 mg of chromium.

6 Apparatus
6.1 General
Ordinary laboratory apparatus and the following.

All volumetric glassware shall be class A and calibrated in accordance with ISO 385, ISO 648 or

ISO 1042, as appropriate.
6.1.1 Polytetrafluoroethylene (PTFE) beakers, of capacity 250 ml.
6.1.2 Polypropylene volumetric flasks, of capacity 100 ml.
6.1.3 Optical emission spectrometer (OES), equipped with ICP.

The spectrometer shall be equipped with a nebulization system. The instrument used will be

satisfactory if, after optimizing in accordance with the manufacturer’s instructions, it meets the

performance requirements given in 6.2.1 to 6.2.5.

The spectrometer can be either a simultaneous or a sequential one. If a sequential spectrometer can be

equipped with an extra arrangement for simultaneous measurement of the internal reference element

line, it can be used with the internal reference element method. If the sequential spectrometer is not

equipped with this arrangement, an internal reference element cannot be used and an alternative

method without an internal reference element should be applied.
6.2 Instrument performance requirements
6.2.1 Wavelengths

This document does not specify particular wavelengths. It is mandatory that each laboratory inve

...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.