Steel -- Determination of Mo, Nb and W contents in alloyed steel -- Inductively coupled plasma atomic emission spectrometric method

ISO/TS 13899-1:2005 specifies a method for the determination of tungsten content in steel by means of inductively coupled plasma atomic emission spectrometry.

Aciers -- Dosage du Mo, du Nb et du W dans les aciers alliés -- Méthode par spectrométrie d'émission atomique avec plasma induit par haute fréquence

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Status
Published
Publication Date
03-Mar-2005
Current Stage
6060 - International Standard published
Start Date
27-Jan-2005
Completion Date
04-Mar-2005
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ISO/TS 13899-3:2005 - Steel -- Determination of Mo, Nb and W contents in alloyed steel -- Inductively coupled plasma atomic emission spectrometric method
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TECHNICAL ISO/TS
SPECIFICATION 13899-3
First edition
2005-02-15
Steel — Determination of Mo, Nb and W
contents in alloyed steel — Inductively
coupled plasma atomic emission
spectrometric method —
Part 3:
Determination of W content
Aciers — Dosage du Mo, du Nb et du W dans les aciers alliés —
Méthode par spectrométrie d'émission atomique avec plasma induit par
haute fréquence —
Partie 3: Dosage du W
Reference number
ISO/TS 13899-3:2005(E)
ISO 2005
---------------------- Page: 1 ----------------------
ISO/TS 13899-3:2005(E)
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ii © ISO 2005 – All rights reserved
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ISO/TS 13899-3:2005(E)
Contents Page

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

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

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

3 Principle................................................................................................................................................. 1

4 Reagents................................................................................................................................................ 2

5 Apparatus.............................................................................................................................................. 3

6 Sampling and samples......................................................................................................................... 4

7 Procedure.............................................................................................................................................. 4

7.1 Preparation of test solution, T ........................................................................................................... 4

7.2 Preparation for spectrometric measurements................................................................................... 5

7.3 Pre-analysis of the test solution.......................................................................................................... 5

7.4 Preparation of calibration solutions for bracketing, K and K .................................................... 6

Ln Hn

7.5 Analysis of test solutions .................................................................................................................... 6

8 Expression of results............................................................................................................................ 6

8.1 Method of calculation ........................................................................................................................... 6

8.2 Precision................................................................................................................................................ 6

9 Test report............................................................................................................................................. 7

Annex A (normative) Procedure for the determination of instrumental criteria.......................................... 8

Annex B (informative) Additional information on the international collaborative trial ............................. 10

Annex C (informative) Graphical representation of precision data............................................................. 12

© ISO 2005 – All rights reserved iii
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ISO/TS 13899-3:2005(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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

In other circumstances, particularly when there is an urgent market requirement for such documents, a

technical committee may decide to publish other types of normative document:

— an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in

an ISO working group and is accepted for publication if it is approved by more than 50 % of the members

of the parent committee casting a vote;

— an ISO Technical Specification (ISO/TS) represents an agreement between the members of a technical

committee and is accepted for publication if it is approved by 2/3 of the members of the committee casting

a vote.

An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed for a

further three years, revised to become an International Standard, or withdrawn. If the ISO/PAS or ISO/TS is

confirmed, it is reviewed again after a further three years, at which time it must either be transformed into an

International Standard or be withdrawn.

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.

ISO/TS 13899-3 was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of

determination of chemical composition.

ISO/TS 13899 consists of the following parts, under the general title Steel — Determination of Mo, Nb and W

contents in alloyed steel — Inductively coupled plasma atomic emission spectrometric method:

 Part 1: Detemination of Mo content
 Part 2: Detemination of Nb content
 Part 3: Detemination of W content
iv © ISO 2005 – All rights reserved
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TECHNICAL SPECIFICATION ISO/TS 13899-3:2005(E)
Steel — Determination of Mo, Nb and W contents in alloyed
steel — Inductively coupled plasma atomic emission
spectrometric method —
Part 3:
Determination of W content
1 Scope

This Technical Specification specifies a method for the determination of tungsten content in steel by means of

inductively coupled plasma atomic emission spectrometry.

This method is applicable to tungsten contents between 0,1 % and 20 % (mass fraction).

2 Normative references

The following referenced documents are indispensable for the application 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 648:1977, Laboratory glassware — One-mark pipettes
ISO 1042:1998, Laboratory glassware — One-mark volumetric flasks

ISO 3696:1987, Water for analytical laboratory use — Specification and test methods

ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results — Part 1: General

principles and definitions

ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic

method for the determination of repeatability and reproducibility of a standard measurement method

ISO 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results — Part 3:

Intermediate measures of the precision of a standard measurement method

ISO 14284:1996, Steel and iron — Sampling and preparation of samples for the determination of chemical

composition
3 Principle

The sample is dissolved in a hydrochloric, nitric and hydrofluoric acid mixture and fumed with a phosphoric

and perchloric acid mixture. Hydrofluoric acid and an internal standard element (if used) are added and the

solution is diluted to known volume. The solution is filtered and nebulized into an inductively coupled plasma

(ICP) spectrometer and the intensity of the emitted light from the element is measured simultaneously with the

light emitted from the internal standard element.
© ISO 2005 – All rights reserved 1
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ISO/TS 13899-3:2005(E)

The method uses a calibration based on close matrix matching of the calibration solutions to the sample and

close bracketing of the tungsten content around the approximate concentration of tungsten in the sample to be

analysed. This compensates for matrix interferences and provides high accuracy, even in highly alloyed steels

where spectral interferences can be severe. Nonetheless, all interferences shall be kept to a minimum and it is

therefore essential that the spectrometer used meets the performance criteria specified in the method for the

selected analytical lines.

In order to accurately matrix match, it is necessary to know the content of all elements in the sample (to the

nearest %). To this end, it may be necessary to carry out a preliminary analysis of the sample by a

semi-quantitative method.
4 Reagents

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

grade 2 water as specified in ISO 3696.
4.1 Hydrofluoric acid, HF, 40 % (mass fraction), ρ approximately 1,14 g/ml
4.2 Hydrochloric acid, HCl, ρ approximately 1,19 g/ml
4.3 Nitric acid, HNO , ρ approximately 1,40 g/ml
4.4 Phosphoric acid, H PO , ρ approximately 1,70 g/ml, diluted 1 + 1
3 4
4.5 Perchloric acid, HClO , ρ approximately 1,54 g/ml, diluted 1 + 1

4.6 Fuming acid mixture: mix 100 ml of the phosphoric acid (4.4) and 300 ml of the perchloric acid (4.5)

4.7 Internal standard solution, 1 000 mg/l

Choose a suitable element to be added as internal standard and prepare a 1 000 mg/l solution. The internal

standard chosen
 shall be pure,
 shall not be present in the sample, and

 shall not interfere with analytical wavelengths, nor should the internal standard element wavelength be

interfered with by elements in the test solution.

The internal standard shall be soluble in the acids used and it shall not cause precipitation. Moreover, the

excitation conditions of the analytical line and the internal standard element line should match.

4.8 Tungsten stock standard solution, 1 000 mg/l

Weigh, to the nearest 0,001 g, 0,5 g of high purity tungsten [minimum 99,95 % (mass fraction)] and dissolve in

a mixture of 10 ml hydrofluoric acid (4.1) and 20 ml nitric acid (4.3). Cool and transfer the solution

quantitatively to a calibrated 500 ml one-mark plastic volumetric flask. Dilute to the mark with water and mix.

1 ml of this solution contains 1 mg of W.

It is not permitted to use pre-prepared tungsten standard solutions supplied by second parties.

4.9 Tungsten standard solution, 100 mg/l

Transfer, with a calibrated micropipette, 25 ml of the tungsten stock standard solution (4.8) into a calibrated

250 ml one-mark plastic volumetric flask. Add 5 ml of hydrofluoric acid (4.1) and 10 ml of nitric acid (4.3).

Dilute to the mark with water and mix. 1 ml of this solution contains 0,1 mg of W.

2 © ISO 2005 – All rights reserved
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ISO/TS 13899-3:2005(E)

NOTE If calibrated micropipettes of suitable volume are not available it would be more advantageous to use more

concentrated standard solutions. These solutions must, however, be prepared for each series of analysis, in order to avoid

possible precipitation.
4.10 Standard solutions of interfering and matrix elements

Prepare standard solutions for each element of which more than 1 % (mass fraction) is contained in the test

sample. Use pure elements or oxides with tungsten contents less than 10 µg/g. Commercial certified standard

solutions can also be used if the tungsten content is less than the value specified above.

NOTE If a large amount of an element is to be added (e.g. iron), it might be more advantageous to use the pure

metal and weigh the correct amount (see 7.3 and 7.4). In this case, use the dissolution procedure described in 7.1.2.

5 Apparatus

The plastic pipettes and flasks to be used shall be calibrated in accordance with ISO 648 or ISO 1042, as

appropriate.
Ordinary laboratory apparatus and

5.1 Atomic emission spectrometer, equipped with an inductively coupled plasma (ICP) and a

nebulization system resistant to hydrofluoric acid.

When a polytetrafluoroethylene (PTFE) nebulizer is used, it is recommended that a surface active agent

should be added to improve wetting in the nebulizer and spray chamber. Modern nebulizers are, however,

often manufactured of plastic materials with better wetting-characteristics than PTFE and can therefore (as is

the case with sapphire nebulizers) be used without a surface active agent.

The ICP-ES spectrometer used will be satisfactory if, after optimising according to 7.2.1 to 7.2.4, it meets the

performance criteria given in 5.1.2 to 5.1.4.

The spectrometer can be either the simultaneous or the sequential type. A sequential type can be used either

with or without an internal standard. However, if a sequential spectrometer is to be used with an internal

standard, it shall be fitted with an arrangement which allows for the simultaneous measurement of the internal

standard line.
5.1.1 Analytical lines

This standard does not specify any particular emission line. It is mandatory that each laboratory carefully

investigates the line/lines available on its own equipment to find the most suitable one regarding sensitivity

and freedom from interferences.
In Table 1, how
...

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