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

ISO/TS 13899-1:2004 specifies an inductively coupled plasma atomic emission spectrometric method for the determination of molybdenum content in steel. The method is applicable to molybdenum contents between 0,03 % (mass fraction) and 8,5 % (mass fraction).

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
31-Mar-2004
Current Stage
6060 - International Standard published
Start Date
10-Mar-2004
Completion Date
01-Apr-2004
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ISO/TS 13899-1:2004 - 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 13899-1
First edition
2004-04-01
Steel — Determination of Mo, Nb and W
contents in alloyed steel — Inductively
coupled plasma atomic emission
spectrometric method —
Part 1:
Determination of Mo 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 1: Dosage du Mo
Reference number
ISO/TS 13899-1:2004(E)
ISO 2004
---------------------- Page: 1 ----------------------
ISO/TS 13899-1:2004(E)
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ii © ISO 2004 – All rights reserved
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ISO/TS 13899-1:2004(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 Determination procedure ..................................................................................................................... 4

7.1 Test portion ........................................................................................................................................... 4

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

7.3 Optimization of spectrometer .............................................................................................................. 4

7.4 Pre-determination of the test solution ................................................................................................ 4

7.5 Preparation of calibration solutions for bracketing, K and K .................................................... 5

Ln Hn

7.6 Determination of test solutions ........................................................................................................... 5

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

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

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

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

Annex A (informative) Suggested analytical lines together with possible spectral interferences in

determination of molybdenum in steel by ICP-AES .......................................................................... 8

Annex B (informative) Additional information on international cooperative tests...................................... 9

Annex C (informative) Graphical representation of precision data............................................................. 11

© ISO 2004 – All rights reserved iii
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ISO/TS 13899-1:2004(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 13899-1 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: Determination of Mo content
 Part 2: Determination of Nb content
 Part 3: Determination of W content
iv © ISO 2004 – All rights reserved
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TECHNICAL SPECIFICATION ISO/TS 13899-1:2004(E)
Steel — Determination of Mo, Nb and W contents in alloyed
steel — Inductively coupled plasma atomic emission
spectrometric method —
Part 1:
Determination of Mo content
1 Scope

This Technical Specification specifies an inductively coupled plasma atomic emission spectrometric method

for the determination of molybdenum content in steel.

The method is applicable to molybdenum contents between 0,03 % (mass fraction) and 8,5 % (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

Dissolution of a test portion in a mixture of hydrochloric, nitric and phosphoric acid and fuming with a mixture

of phosphoric and perchloric acids. Addition of hydrofluoric acid and, if necessary, an internal reference

element and dilution of the solution to known volume. Nebulization of the solution into an inductively coupled

plasma atomic emission spectrometer and measurement of the intensity of the emitted light from molybdenum,

or with emitted light from the internal reference element, simultaneously.
© ISO 2004 – All rights reserved 1
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ISO/TS 13899-1:2004(E)

NOTE 1 The method uses a calibration graph based on a very close matrix matching of the calibration solutions to the

sample and close bracketing of the contents around the approximate concentration of molybdenum in the sample to be

analysed. The concentrations of all elements in the sample must, therefore, be approximately known. If the concentrations

are not known, the sample must be analysed by some semi-quantitative method.

NOTE 2 The advantage with this procedure is that all possible interferences from the matrix are automatically

compensated, which results in high accuracy. This is most important for spectral interferences, which can be severe in

very highly alloyed steels. However, all possible interferences must be kept on a minimum level. Therefore it is essential

that the spectrometer used meets the performance criteria specified in the method for the selected analytical lines.

Examples of the analytical lines are given in Table 1.
Table 1 — Examples of analytical lines together with interfering elements
Analytical line
Element Interferences
202,03 Ta
Molybdenum
281,61 Al, Hf

NOTE 3 These lines have been carefully investigated (see Annex A). The strongest possible interferences are given in

Table 1. If other lines are used, they have to be carefully checked so that interferences are not higher than the values

given in Annex A. It is recommended to use scandium 363.07 nm. This line is interference-free for the elements and

concentrations given in Annex A.
4 Reagents

During the analysis, unless otherwise stated, use only reagents of recognized 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, or 50 % (mass fraction), ρ

approximately 1,17 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 Internal standard solution, 1 000 mg/l

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

4.7 Molybdenum stock standard solution, 1 000 mg/l

Weigh, to the nearest 0,000 5 g, 0,5 g of high purity molybdenum [minimum 99,95 % (mass fraction)] and

dissolve in a mixture of 25 ml hydrochloric acid (4.2) and 25 ml nitric acid (4.3). Keep the temperature of a

one-mark volumetric flask the same as that at which the volumetric flask was calibrated. Cool and transfer the

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

4.8 Molybdenum standard solution, 100 mg/l

Keep the temperature of a one-mark volumetric flask the same as that at which the volumetric flask was

calibrated. Using a calibrated pipette, transfer 100 ml of the molybdenum stock standard solution (4.7) into a

2 © ISO 2004 – All rights reserved
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ISO/TS 13899-1:2004(E)

calibrated 1 000 ml one-mark volumetric flask. Add 10 ml of hydrochloric acid (4.2). Dilute to the mark with

water and mix.
4.9 Molybdenum standard solution, 10 mg/l

Keep the temperature of a one-mark volumetric flask the same as that at which the volumetric flask was

calibrated. Using a calibrated pipette, transfer 100 ml of the molybdenum standard solution (4.8) into a

calibrated 1 000 ml one-mark volumetric flask. Add 10 ml of hydrochloric acid (4.2). Dilute to the mark with

water and mix.
4.10 Standard solutions of interfering elements

Prepare standard solutions for each element of which more than 1 % by mass is contained in the test sample.

Use pure metal or chemical substances with molybdenum contents less
...

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