GB/T 6730.87-2023 English PDF (GBT6730.87-2023)

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GB/T 6730.87-2023: Iron ores - Determination of total iron and other multi-element content - Wavelength dispersive X-ray fluorescence spectrometry (cobalt internal standard method)
GB/T 6730.87-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060.10
CCS D 31
Iron ores - Determination of total iron and other multi-
element content - Wavelength dispersive X-ray fluorescence
spectrometry (cobalt internal standard method)
ISSUED ON: AUGUST 06, 2023
IMPLEMENTED ON: MARCH 01, 2024
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword ... 3
Introduction ... 4
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions ... 6
4 Principle ... 6
5 Reagents and materials ... 6
6 Instruments and equipment ... 8
7 Sampling and sample preparation ... 9
8 Preparation of glass pieces ... 9
9 Instrument preparation ... 13
10 Analysis steps ... 13
11 Result calculation and representation ... 17
12 Test report ... 21
Annex A (informative) Parts of GB/T 6730 that have been published ... 22
Annex B (normative) Procedure for acceptance of specimen analysis results ... 27
Annex C (informative) Raw data from precision tests ... 28
Iron ores - Determination of total iron and other multi-
element content - Wavelength dispersive X-ray fluorescence
spectrometry (cobalt internal standard method)
WARNING -- Personnel using this document shall have practical experience in
formal laboratory work. This document does not identify all possible security
issues. Users are responsible for taking appropriate safety and health measures
and ensuring compliance with relevant national regulations.
1 Scope
This document specifies the use of wavelength dispersive X-ray fluorescence
spectrometry (cobalt internal standard method) for the determination of all iron, silicon,
aluminum, calcium, magnesium, manganese, titanium, vanadium, phosphorus, copper,
lead, chromium, zinc, arsenic, potassium and sulfur content.
This document is applicable to the determination of the following elements in iron ore,
iron concentrate, sinter and pellets. The measurement range is shown in Table 1.
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.
GB/T 6682, Water for analytical laboratory use -- Specification and test methods
GB/T 6730.1, Iron ores -- Preparation of pre-dried test samples for chemical
analysis
GB/T 8170, Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 10322.1, Iron ores - Sampling and sample preparation procedures
GB/T 15000.3, Directives for the work of reference materials -- Part 3: Reference
materials -- Characterization and assessment of homogeneity and stability
GB/T 16597, Analytical methods of metallurgical products -- General rule for X-ray
fluorescence spectrometric methods
JJG 810, Verification Regulation for Wavelength Dispersive X-Ray Fluorescence
Spectrometers
YB/T 082, Specification for certified reference materials for metallurgical product
analysis
3 Terms and definitions
There are no terms or definitions to be defined in this document.
4 Principle
The sample and the cobalt internal standard added accurately in quantitative amounts
are melted into a borate glass piece with the flux. Measure the X-ray fluorescence
intensity of the element to be measured. Use the X-ray fluorescence intensity of the
element to be measured (iron/cobalt X-ray fluorescence intensity ratio) to establish a
calibration curve for the content of the element to be measured. Calculate the content
of the element to be measured based on the calibration curve.
5 Reagents and materials
Unless otherwise stated, only approved analytically pure reagents and grade 3 or above
distilled water complying with GB/T 6682 or water with equivalent purity are used in
the analysis.
5.1 Iron dioxide (Fe2O3), guaranteed reagent. Burn ferric oxide at 1000°C for at least 1
h and cool to room temperature in a desiccator.
5.2 Copper oxide (CuO), guaranteed reagent. Burn copper oxide at 400°C for at least 1
h and cool to room temperature in a desiccator.
5.3 Zinc oxide (ZnO), guaranteed reagent. Burn zinc oxide at 400°C for at least 1 h and
cool to room temperature in a desiccator.
5.4 Lead oxide (PbO), guaranteed reagent. Burn lead oxide at 400°C for at least 1 h and
cool to room temperature in a desiccator.
5.5 Arsenic trioxide (As2O3), guaranteed reagent. Bake arsenic trioxide at 105°C for at
least 1 h and cool to room temperature in a desiccator.
5.6 Chromium trioxide (Cr2O3), guaranteed reagent. Burn chromium trioxide at 400°C
for at least 1 h and cool to room temperature in a desiccator.
5.7 Silica (SiO2), guaranteed reagent. Burn silica at 1000°C for at least 1 h and cool to
room temperature in a desiccator.
5.8 Calcium carbonate (CaCO3), guaranteed reagent. Bake calcium carbonate at 105°C
for at least 1 hour and cool to room temperature in a desiccator.
5.9 Magnesium oxide (MgO), guaranteed reagent. Burn magnesium oxide at 1000°C
for at least 1 h and cool to room temperature in a desiccator. Weigh immediately.
5.10 Aluminum trioxide (Al2O3), guaranteed reagent. Ignite aluminum oxide at 1000°C
for at least 2 h and cool to room temperature in a desiccator.
5.11 Manganese tetroxide (Mn3O4), guaranteed reagent. Bake manganese tetroxide at
105°C for at least 2 h and cool to room temperature in a desiccator.
5.12 Ammonium dihydrogen phosphate (NH4H2PO4), guaranteed reagent. Bake
ammonium dihydrogen phosphate at 105°C for at least 1 h and cool to room temperature
in a desiccator.
5.13 Potassium carbonate (K2CO3), guaranteed reagent. Bake potassium carbonate at
105°C for at least 1 h and cool to room temperature in a desiccator.
5.14 Titanium dioxide (TiO2), guaranteed reagent. Burn the titanium dioxide at 1000°C
for at least 1 h and cool to room temperature in a desiccator.
5.15 Vanadium pentoxide (V2O5), guaranteed reagent. Bake vanadium pentoxide at
110°C for at least 1 h and cool to room temperature in a desiccator.
5.16 Ammonium sulfate [(NH4)2SO4], guaranteed reagent. Bake ammonium sulfate at
105°C for at least 1 h and cool to room temperature in a desiccator.
5.17 Lithium carbonate (Li2CO3), guaranteed reagent.
5.18 Cobalt trioxide (Co2O3). Bake cobalt oxide at 105°C for at least 1 h and cool to
room temperature in a desiccator.
5.19 Anhydrous lithium tetraborate (Li2B4O7), guaranteed reagent.
7 Sampling and sample preparation
7.1 Laboratory specimens
Samples shall be taken and prepared in accordance with the provisions of GB/T 10322.1.
The particle size of the specimen shall be less than 100 μm. If the content of combined
water or easy oxides in the specimen is high, the particle size shall be less than 160 μm.
For regulations regarding high combined water and easy oxide content, see GB/T
6730.1.
7.2 Preparation of pre-dried specimens
Prepare pre-dried specimens according to the provisions of GB/T 6730.1.
8 Preparation of glass pieces
8.1 General
When preparing glass pieces, the weighing amount of the test material is 0.4 g~0.8 g,
accurate to 0.0001 g. The amount of flux used is 10 ~ 15 times the test material amount.
The flux can be a single commercially available lithium tetraborate or a mixture of
lithium tetraborate, lithium metaborate, and lithium carbonate [the ratio (mass fraction)
of lit...