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GB/T 6730.87-2023 PDF English

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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)
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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)


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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

Foreword

This document was drafted in accordance with the rules given in GB/T 1.1-2020 "Directives for standardization - Part 1.Rules for the structure and drafting of standardizing documents". This document is Part 87 of GB/T 6730 "Iron ores". See Annex A for the published parts of GB/T 6730. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. The issuing authority shall not be held responsible for identifying any or all such patent rights. This document was proposed by China Iron and Steel Industry Association. This document shall be under the jurisdiction of National Technical Committee on Iron Ores and Direct Reduced Irons of Standardization Administration of China (SAC/TC 317). Main drafting organizations of this document. Wuhan University of Science and Technology, Jiangsu Shagang Group Co., Ltd., Guangxi Liuzhou Iron and Steel Group Co., Ltd., Guangdong Zhongnan Iron and Steel Co., Ltd., Jiangsu Yonggang Group Co., Ltd., Hunan Valin Lianyuan Iron and Steel Co., Ltd., Zhongxin Iron and Steel Group Co., Ltd., Panxi Vanadium Titanium Inspection and Testing Institute, Metallurgical Industry Information Standards Institute. Main drafters of this document. Zhou Shuangqing, Zhu Qingyou, Xu Jianping, Zhang Jiming, Zhu Chunyao, Li Jiao, Huang Zhimin, Xing Wenqing, Yu Lei, Zhao Jie, Chen Haiyan, Wu Yuan, Xiao Xing, Zhuo Wenkeng, Zhang Zhongting, Li Zijing, Sun Hao, Chen Zibin, Zhu Rong, Li Shijing, Zhu Zhijin, Wu Chaochao.

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 Element Element Measurement range (mass fraction) % Measurement range (mass fraction) % 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.

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. 5.8 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. 5.22 Ammonium bromide (NH4Br) solution, 300 g/L. Dissolve 15.0 g of ammonium bromide in 50 mL of water. 5.23 Ammonium iodide (NH4I) solution, 300 g/L. Dissolve 15.0 g of ammonium iodide in 50 mL of water. 5.24 Standard samples/standard materials. They are used for establishing calibration curves and quality control. The selected standard samples/standard materials shall comply with the regulations of GB/T 15000.3 and YB/T 082.The content of each analyzed element shall cover the analysis range and have an appropriate gradient.

6 Instruments and equipment

6.1 Wavelength dispersive X-ray fluorescence spectrometer The X-ray fluorescence spectrometer shall meet the requirements of JJG 810 and GB/T 16597. 6.2 Analytical balance The accuracy is 0.1 mg. 6.4 Melting furnace Electrically heated, high frequency heated or gas heated melting furnace. The maximum working temperature is not less than 1100℃. Temperature control accuracy is ±10℃. 6.5 Crucible and mold (or crucible doubles as mold) The crucible is made of platinum-gold alloy (95% Pt.5% Au) and has a volume sufficient to accommodate the weighed flux and test material. The mold shall be thick enough to prevent deformation after heating.

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 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. 8.2 Preparation of glass pieces for calibration 8.2.1 Preparation of synthetic calibration samples Take the appropriate amount of the pure substance corresponding to the component being determined based on the conventional high-point content of the component being determined. 8.2.4 Preparation of standard samples/standard substance glass pieces The preparation method of glass pieces for calibration using standard samples/standard substances shall be consistent with the preparation method of glass pieces for sample measurement. 8.2.5 Preparation of standard samples/standard substances by adding pure substances to glass pieces Weigh the weighing amount of standard sample/standard substance and pure substance calculated based on the molecular formula of the pure substance and the measured component. Melt the glass piece for calibration. 8.3 Pre-oxidize and then melt lithium tetraborate flux base 8.4 Pre-oxidize and then melt in an internal standard flux crucible 8.4.1 Weigh 1.00 g of lithium carbonate (see 5.17) (accurate to 0.01 g) and 0.5000 g of test material (accurate to 0.0001 g). Place in a 50 mL clean glass beaker. Mix well. Transfer to a crucible containing internal standard flux (see 5.21). Add 0.15 mL~0.25 mL of ammonium bromide solution (see 5.22) [note that Br interferes with Al and shall be calibrated, or add 0.2 mL~1.0 mL of ammonium iodide solution (see 5.23)] to the mixture of lithium carbonate and test material. 8.4.2 Transfer the internal standard flux crucible (see 5.21) and the materials in it to a crucible (see 6.5) with a mass of m1 (accurate to 0.0001 g) after constant weight. Weigh 1.70 g of anhydrous lithium tetraborate (see 5.19) and cover it on the mixture of test material, lithium carbonate and release agent. 8.5 Pre-oxidize and then melt boric acid 8.5.1 Take 3.01 g of anhydrous boric acid (see 5.20) (accurate to 0.01 g), 0.5000 g of test material (accurate to 0.0001 g), 0.1000 g of cobalt trioxide (see 5.18) (accurate to 0.0001 g). 8.6 Pre-oxidize and then melt in a cobalt-containing internal standard flux crucible - add boric acid 8.6.1 Weigh 1.00 g of lithium carbonate (see 5.17) (accurate to 0.01 g) and 0.5000 g of test material (accurate to 0.0001 g). Place in a 50 mL clean glass beaker. Mix well. Transfer to a crucible containing internal standard flux (see 5.21). Add 0.15 mL~0.25 mL of ammonium bromide solution (see 5.22) [Note that Br interferes with Al and shall be calibrated, or add 0.2 mL~1.0 mL of ammonium iodide solution (see 5.23)] to the mixture of lithium carbonate and test material. 8.6.2 Transfer the internal standard flux crucible (see 5.21) and its contents to a clean ceramic crucible cover. And move it into a high temperature furnace of 450℃±10℃ (see 6.3). Raise the temperature to 500°C and keep it for 20 min. Then the temperature is raised to 600°C and kept for 20 min. Finally, the temperature is raised to 650°C and maintained for 20 min. Take it out after completing pre-oxidation.

9 Instrument preparation

9.1 Instrument working environment The working environment of the instrument shall meet the requirements of GB/T 16597. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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