GB/T 15617-2025 Microbeam analysis—Electron probe microanalysis—Quantitative analysis of silicate minerals English, Anglais, Englisch, Inglés, えいご
This is a draft translation for reference among interesting stakeholders. The finalized translation (passing through draft translation, self-check, revision and verification) will be delivered upon being ordered.
ICS 71.040.99
CCS H 57
National Standard of the People's Republic of China
GB/T 15617-2025
Replaces GB/T 15617-2002
Microbeam analysis - Electron probe mieroanalysis - Quantitative analysis of silicate minerals
Issue date: 2025-08-29 Implementation date: 2026-03-01
Issued by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
the Standardization Administration of the People's Republic of China
Contents
Foreword
Introduction
1 Scope
2 Normative References
3 Terms and Definitions
4 Instruments and Auxiliary Equipment
5 Reference Materials/Standard Samples
6 Test Portions
7 Measurement Conditions
8 Analytical Procedure
9 Permissible Error
10 Reporting of Analytical Results
Microbeam analysis - Electron probe mieroanalysis - Quantitative analysis of silicate minerals
1 Scope
This document describes the quantitative analysis method for natural silicate minerals stable under electron beam irradiation using electron probe microanalysis (EPMA).
This document is applicable to:
Natural silicate minerals; Artificial synthetic silicate materials; Other oxygen-containing salts, such as phosphates and sulfates; Oxide minerals and materials.
This document is applicable to quantitative analysis using EPMA and scanning electron microscopes equipped with wavelength-dispersive spectrometers (WDS).
2 Normative References
The following documents contain provisions that, through reference in this text, constitute essential requirements of this document. For dated references, only the cited version applies. For undated references, the latest version (including any amendments) applies.
GB/T 4930: Microbeam Analysis – Electron Probe Microanalysis – Guidelines for Reference Material Specifications
GB/T 15074: General Principles for Quantitative Analysis by Electron Probe Microanalysis
GB/T 17366: Preparation Methods for Samples of Mineral Rocks for Electron Probe Microanalysis
GB/T 20725: Guidelines for Qualitative Spot Analysis by Electron Probe Microanalysis using WDS
GB/T 21636: Microbeam Analysis – Electron Probe Microanalysis (EPMA) – Terminology
GB/T 43889: Microbeam Analysis – Electron Probe Microanalysis (EPMA) – Guidelines for Quality Assurance Program Implementation
3 Terms and Definitions
Terms and definitions in GB/T 21636 and GB/T 43889 apply to this document.
4 Instruments and Auxiliary Equipment
Electron probe microanalyzer or scanning electron microscope with WDS;
Sample grinder and polisher;
Vacuum coater;
Ultrasonic cleaner;
Polarizing microscope.
5 Reference Materials/Standard Samples
5.1 Selection Principles
5.1.1 Certified reference materials (CRMs) or standard samples should be used when available. If no suitable CRMs are available, alternative reference materials may be selected per GB/T 4930.
5.1.2 reference materials with similar composition and structure to the sample should be selected (e.g., same mineral type).
5.1.3 The mass fraction of the element used as a standard in the reference material should preferably be equal to or higher than that in the sample.
5.2 Commonly Used Reference Materials
5.2.1 Silicate mineral reference materials: Olivine, pyroxene, potassium feldspar, albite, jadeite, kyanite, wollastonite, nosean, titanite, chromite, rhodonite, etc. Other oxygen-containing salt reference materials: Apatite, barite, potassium niobate, manganotantalite, mimetite, etc.
5.2.2 Oxide mineral reference materials: Periclase (MgO), corundum (Al₂O₃), quartz (SiO₂), rutile (TiO₂), hematite (Fe₂O₃), manganosite (MnO), cassiterite (SnO₂), etc. Synthetic oxide reference materials: Cr₂O₃, CoO, NiO, ZnO, Cu₂O, TeO₂, etc.
6 Sample Preparation
6.1 Sample Preparation
6.1.1 Sample preparation shall be conducted per GB/T 17366.
6.1.2 Samples may be prepared as polished sections, thin sections, or lapped sections using grinders and polishers. Where possible, samples should be prepared as thin sections (~30 μm thick) to facilitate optical observation under a polarizing microscope.
6.1.3 Adhesives should be vacuum- and electron beam-stable (e.g., epoxy resin). Final polishing should use diamond paste with particle size <1 μm to ensure a smooth surface.
6.1.4 Samples should be cleaned in distilled or deionized water using an ultrasonic cleaner to remove contaminants.
6.2 Selection and Marking of Analytical Positions
6.2.1 Samples should be examined under an optical microscope to select and mark analytical positions. Photos or sketches may be taken if necessary.
6.2.2 The grain size of the mineral to be analyzed should preferably be >5 μm. The analytical area should be free of inclusions, scratches, or cleavage and should avoid mineral boundaries.
6.3 Coating
6.3.1 Silicate samples should be coated with carbon. Ensure the sample surface is clean and dry before coating.
6.3.2 Coating thickness should match that of the reference material (~20 nm). If the coater cannot control thickness, use interference colors on a brass-polished surface (blue-purple at ~20 nm) or a set of reference ceramic plates with varying carbon thicknesses for real-time monitoring.
6.3.3 Coated samples should be stored in a desiccator.
7 Measurement Conditions
7.1 Accelerating Voltage: 15 kV or 20 kV.
7.2 Beam Current: 20 nA (adjustable based on element content and count rate).
7.3 Beam Spot Size: 1–10 μm (smaller for fine grains; larger for beam-sensitive samples, e.g., 10–50 μm).
7.4 X-ray Selection:
K-lines for elements with Z < 32;
L-lines for Z = 32–72;
M-lines for Z > 72.
Choose high-resolution and high-efficiency crystals while optimizing element allocation.
7.5 Counting Time:
10–20 s for major elements (>5%);
GB/T 15617-2025 Microbeam analysis—Electron probe microanalysis—Quantitative analysis of silicate minerals English, Anglais, Englisch, Inglés, えいご
This is a draft translation for reference among interesting stakeholders. The finalized translation (passing through draft translation, self-check, revision and verification) will be delivered upon being ordered.
ICS 71.040.99
CCS H 57
National Standard of the People's Republic of China
GB/T 15617-2025
Replaces GB/T 15617-2002
Microbeam analysis - Electron probe mieroanalysis - Quantitative analysis of silicate minerals
Issue date: 2025-08-29 Implementation date: 2026-03-01
Issued by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
the Standardization Administration of the People's Republic of China
Contents
Foreword
Introduction
1 Scope
2 Normative References
3 Terms and Definitions
4 Instruments and Auxiliary Equipment
5 Reference Materials/Standard Samples
6 Test Portions
7 Measurement Conditions
8 Analytical Procedure
9 Permissible Error
10 Reporting of Analytical Results
Microbeam analysis - Electron probe mieroanalysis - Quantitative analysis of silicate minerals
1 Scope
This document describes the quantitative analysis method for natural silicate minerals stable under electron beam irradiation using electron probe microanalysis (EPMA).
This document is applicable to:
Natural silicate minerals; Artificial synthetic silicate materials; Other oxygen-containing salts, such as phosphates and sulfates; Oxide minerals and materials.
This document is applicable to quantitative analysis using EPMA and scanning electron microscopes equipped with wavelength-dispersive spectrometers (WDS).
2 Normative References
The following documents contain provisions that, through reference in this text, constitute essential requirements of this document. For dated references, only the cited version applies. For undated references, the latest version (including any amendments) applies.
GB/T 4930: Microbeam Analysis – Electron Probe Microanalysis – Guidelines for Reference Material Specifications
GB/T 15074: General Principles for Quantitative Analysis by Electron Probe Microanalysis
GB/T 17366: Preparation Methods for Samples of Mineral Rocks for Electron Probe Microanalysis
GB/T 20725: Guidelines for Qualitative Spot Analysis by Electron Probe Microanalysis using WDS
GB/T 21636: Microbeam Analysis – Electron Probe Microanalysis (EPMA) – Terminology
GB/T 43889: Microbeam Analysis – Electron Probe Microanalysis (EPMA) – Guidelines for Quality Assurance Program Implementation
3 Terms and Definitions
Terms and definitions in GB/T 21636 and GB/T 43889 apply to this document.
4 Instruments and Auxiliary Equipment
Electron probe microanalyzer or scanning electron microscope with WDS;
Sample grinder and polisher;
Vacuum coater;
Ultrasonic cleaner;
Polarizing microscope.
5 Reference Materials/Standard Samples
5.1 Selection Principles
5.1.1 Certified reference materials (CRMs) or standard samples should be used when available. If no suitable CRMs are available, alternative reference materials may be selected per GB/T 4930.
5.1.2 reference materials with similar composition and structure to the sample should be selected (e.g., same mineral type).
5.1.3 The mass fraction of the element used as a standard in the reference material should preferably be equal to or higher than that in the sample.
5.2 Commonly Used Reference Materials
5.2.1 Silicate mineral reference materials: Olivine, pyroxene, potassium feldspar, albite, jadeite, kyanite, wollastonite, nosean, titanite, chromite, rhodonite, etc. Other oxygen-containing salt reference materials: Apatite, barite, potassium niobate, manganotantalite, mimetite, etc.
5.2.2 Oxide mineral reference materials: Periclase (MgO), corundum (Al₂O₃), quartz (SiO₂), rutile (TiO₂), hematite (Fe₂O₃), manganosite (MnO), cassiterite (SnO₂), etc. Synthetic oxide reference materials: Cr₂O₃, CoO, NiO, ZnO, Cu₂O, TeO₂, etc.
6 Sample Preparation
6.1 Sample Preparation
6.1.1 Sample preparation shall be conducted per GB/T 17366.
6.1.2 Samples may be prepared as polished sections, thin sections, or lapped sections using grinders and polishers. Where possible, samples should be prepared as thin sections (~30 μm thick) to facilitate optical observation under a polarizing microscope.
6.1.3 Adhesives should be vacuum- and electron beam-stable (e.g., epoxy resin). Final polishing should use diamond paste with particle size <1 μm to ensure a smooth surface.
6.1.4 Samples should be cleaned in distilled or deionized water using an ultrasonic cleaner to remove contaminants.
6.2 Selection and Marking of Analytical Positions
6.2.1 Samples should be examined under an optical microscope to select and mark analytical positions. Photos or sketches may be taken if necessary.
6.2.2 The grain size of the mineral to be analyzed should preferably be >5 μm. The analytical area should be free of inclusions, scratches, or cleavage and should avoid mineral boundaries.
6.3 Coating
6.3.1 Silicate samples should be coated with carbon. Ensure the sample surface is clean and dry before coating.
6.3.2 Coating thickness should match that of the reference material (~20 nm). If the coater cannot control thickness, use interference colors on a brass-polished surface (blue-purple at ~20 nm) or a set of reference ceramic plates with varying carbon thicknesses for real-time monitoring.
6.3.3 Coated samples should be stored in a desiccator.
7 Measurement Conditions
7.1 Accelerating Voltage: 15 kV or 20 kV.
7.2 Beam Current: 20 nA (adjustable based on element content and count rate).
7.3 Beam Spot Size: 1–10 μm (smaller for fine grains; larger for beam-sensitive samples, e.g., 10–50 μm).
7.4 X-ray Selection:
K-lines for elements with Z < 32;
L-lines for Z = 32–72;
M-lines for Z > 72.
Choose high-resolution and high-efficiency crystals while optimizing element allocation.
7.5 Counting Time:
10–20 s for major elements (>5%);
