ISO/TS 9516-4:2021

TECHNICAL ISO/TS
SPECIFICATION 9516-4
First edition
2021-11
Iron ores — Determination of various
elements by X-ray fluorescence
spectrometry —
Part 4:
Performance-based method using
fusion preparation method
Reference number
© ISO 2021
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ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Reagents and materials . 2
4.1 Pure reagents . 2
4.2 Flux . 3
4.3 Releasing agent . 3
4.4 Oxidizing agents . 3
4.5 Certified reference materials . 3
4.6 Reference materials . 3
5 Sampling and samples . .3
5.1 Laboratory sample . 3
5.2 Preparation of test samples, CRMs and RMs . 4
5.2.1 General . 4
5.2.2 Ores having significant contents of combined water or easily oxidizable
compounds . 4
5.2.3 Ores outside the scope of 5.2.2 . 4
5.3 Test portion . 4
6 Apparatus . 4
7 Measurements .5
7.1 General . 5
7.1.1 Analytical line . 5
7.1.2 Voltage and current . 6
7.1.3 Measuring times . 6
7.1.4 Background measurements. 6
8 Calibration and validation .6
8.1 Principles . 6
8.2 Preparation of fusion beads . 6
8.3 Calibration and validation samples . 6
8.4 Validation of the calibration . 7
8.4.1 Specimens . 7
8.4.2 Trueness validation . . 7
8.5 Calibration maintenance . 8
8.5.1 Monitor disc . 8
8.5.2 Duplicate monitor discs . 8
8.5.3 Monitor measurements . 8
8.5.4 Quality control measurements . 9
9 Reporting .10
9.1 General . 10
9.2 Calculation of results . 10
9.3 Number of decimals . 11
10 Test report .11
Bibliography .12
iii
Foreword
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electrotechnical standardization.
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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
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www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron,
Subcommittee SC 2 Chemical analysis.
A list of all parts in the ISO 9516 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
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iv
Introduction
X-ray fluorescence (XRF) spectrometry is a multi-elemental non-destructive analytical methodology
used for quantitative and qualitative determinations. It is element specific covering an elemental range
from boron (B) to uranium (U).
Once the sample has been dissolved into a borate glass it may be introduced to the spectrometer for
analysis. The sample is then irradiated by intense radiation from an X-ray tube. Analysis of fused glass
beads offers advantages over pressed powder techniques as it eliminates particle size effects, and it
produces a homogeneous specimen for each element.
In some instances, the relationship between intensity (or intensity ratios) and concentration can
be linear. For most analytes there is no direct straightforward relationship between intensity and
concentration. With samples of differing compositions, the X-rays are absorbed differently in the
different samples giving rise to what are generally referred to as matrix effects. These inter-element
effects can be corrected using mathematical models derived from the known physics of X-rays.
Calibration can be based on binary standards (prepared from pure oxides or liquid solutions), reference
materials, secondary standards, or combinations therewith.
v
TECHNICAL SPECIFICATION ISO/TS 9516-4:2021(E)
Iron ores — Determination of various elements by X-ray
fluorescence spectrometry —
Part 4:
Performance-based method using fusion preparation
method
WARNING — This document can involve hazardous materials, operations and equipment. This
document does not purport to address all of the safety problems associated with its use. It is the
responsibility of the user of this document to establish appropriate health and safety practices
and determine the applicability of regulatory limitations prior to use.
1 Scope
This document specifies a performance-based method for the chemical analysis of natural and
processed iron ores by fused bead wavelength and energy dispersive X-ray fluorescence (XRF).
It is applicable to all elements of interest when adequate calibrations have been established.
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
...