GB/T 6730.84-2023 (GB/T6730.84-2023, GBT 6730.84-2023, GBT6730.84-2023) & related versions
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Iron ores - Determination of total rare earth content - Inductively coupled plasma atomic emission spectrometric method
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GB/T 6730.84-2023
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GBT 6730.84-2023
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GB/T 6730.84-2023: PDF in English (GBT 6730.84-2023)
GB/T 6730.84-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060.10
CCS D 31
Iron ores - Determination of total rare earth content -
Inductively coupled plasma atomic emission spectrometric
method
ISSUED ON: AUGUST 06, 2023
IMPLEMENTED ON: MARCH 01, 2024
Issued by: State Administration for Market Regulation.
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
Introduction ... 4
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions ... 6
4 Principles ... 6
5 Reagents and materials ... 6
6 Instruments and equipment ... 10
7 Sampling and specimen preparation ... 10
8 Analytical procedures ... 10
9 Result calculation and representation ... 13
10 Test report ... 16
Appendix A (Informative) Released Parts of GB/T 6730 ... 17
Appendix B (Normative) Procedure for acceptance of specimen analysis results ... 22
Appendix C (Informative) Precision test raw data ... 23
Iron ores - Determination of total rare earth content -
Inductively coupled plasma atomic emission spectrometric
method
Warning - Personnel using this document shall have practical experience in
regular laboratory work. This document does not identify all possible safety issues.
Users are responsible for taking appropriate safety and health measures and
ensuring compliance with the conditions, which are stipulated in relevant national
regulations.
1 Scope
This document describes a method for the determination of total rare earth content, by
inductively coupled plasma atomic emission spectrometry.
This document is applicable to the determination of the total rare earth content in iron
ore, iron concentrate, sinter, pellet mineral products. Determination range (mass
fraction): 0.10% ~ 15.00%.
2 Normative references
The contents of the following documents constitute essential provisions of this
document through normative references in the text. Among them, for dated reference
documents, only the version corresponding to the date applies to this document; for
undated reference documents, the latest version (including all amendments) applies to
this document.
GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and
results - Part 1: General principles and definitions
GB/T 6379.2 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
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 & expression and judgement
of limiting values
5.8 Hydrochloric acid, 5 + 95.
5.9 Nitric acid, ρ≈1.42 g/mL.
5.10 Nitric acid, 1 + 1.
5.11 Hydrogen peroxide, 30%.
5.12 Sodium hydroxide lotion, 20 g/L.
Weigh 2 g of sodium hydroxide. Dissolve it in 100 mL of water.
5.13 Triethanolamine, 5 + 95.
Measure 5 mL of triethanolamine. Add 95 mL of water. Mix well.
5.14 Yttrium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of yttrium oxide [w (Y2O3/REO) ≥ 99.99%, w (REO) ≥ 99.5%] that
has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of
hydrochloric acid (see 5.7). Heat at low temperature to dissolve it completely. Cool to
room temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the
mark. Mix well.
5.15 Lanthanum oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of lanthanum oxide [w (La2O3/REO) ≥ 99.99%, w (REO) ≥ 99.5%]
that has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of
hydrochloric acid (see 5.7). Heat at low temperature to dissolve it completely. Cool to
room temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the
mark. Mix well.
5.16 Cerium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of cerium oxide [w (CeO2/REO) ≥ 99.99%, w (REO) ≥ 99.5%] that has
been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of nitric acid
(see 5.10). Heat at low temperature. Dropwise add hydrogen peroxide (see 5.11), until
it is completely dissolved. Cool to room temperature. Transfer to a 100 mL volumetric
flask. Use water to dilute it to the mark. Mix well.
5.17 Praseodymium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of praseodymium oxide [w (Pr6O11/REO) ≥ 99.99%, w (REO) ≥ 99.5%]
that has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of
hydrochloric acid (see 5.7). Heat at low temperature to dissolve it completely. Cool to
room temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the
mark. Mix well.
5.18 Neodymium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of neodymium oxide [w (Nd2O3/REO) ≥ 99.99%, w (REO) ≥ 99.5%]
that has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of
hydrochloric acid (see 5.7). Heat at low temperature to dissolve it completely. Cool to
room temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the
mark. Mix well.
5.19 Samarium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of samarium oxide [w (Sm2O3/REO) ≥ 99.99%, w (REO) ≥ 99.5%]
that has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of
hydrochloric acid (see 5.7). Heat at low temperature to dissolve it completely. Cool to
room temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the
mark. Mix well.
5.20 Europium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of europium oxide [w (Eu2O3/REO) ≥ 99.99%, w (REO) ≥ 99.5%] that
has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of
hydrochloric acid (see 5.7). Heat at low temperature to dissolve it completely. Cool to
room temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the
mark. Mix well.
5.21 Gadolinium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of gadolinium oxide [w (Gd2O3/REO) ≥ 99.99%, w (REO) ≥ 99.5%]
that has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of
hydrochloric acid (see 5.7). Heat at low temperature to dissolve it completely. Cool to
room temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the
mark. Mix well.
5.22 Terbium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of terbium oxide [w (Tb4O7/REO) ≥ 99.99%, w (REO) ≥ 99.5%] that
has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of nitric
acid (see 5.10). Heat at low temperature to dissolve it completely. Cool to room
temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the mark.
Mix well.
5.23 Dysprosium oxide standard storage solution, 1 mg/mL.
Weigh 0.1000 g of dysprosium oxide [w (Dy2O3/REO) ≥ 99.99%, w (REO) ≥ 99.5%]
that has been burned at 950 °C for 1 hour. Place it in a 100 mL beaker. Add 10 mL of
hydrochloric acid (see 5.7). Heat at low temperature to dissolve it completely. Cool to
room temperature. Transfer to a 100 mL volumetric flask. Use water to dilute it to the
mark. Mix well.
6 Instruments and equipment
Unless otherwise specified, use usual laboratory equipment. Single-marked volumetric
flasks, graduated pipettes, single-marked pipettes shall comply with the requirements
of GB/T 12806, GB/T 12807, GB/T 12808, respectively. Corundum crucibles, beakers,
volumetric flasks, etc., which are used in the test, are soaked in hydrochloric acid
solution (see 5.8) for more than 24 hours, rinsed with water, dried, prepared for use.
6.1 Inductively coupled plasma atomic emission spectrometer shall meet the following
requirements:
a) The resolution is less than 0.008 nm (at 200 nm);
b) Comply with the emission spectrometer calibration procedures and technical
indicators required in JJG 768.
6.2 Electric hot plate: Temperature control range 50 °C ~350 °C.
6.3 Muffle furnace: Temperature control range 500 °C ~800 °C.
6.4 Analytical balance: Sensitivity 0.1 mg.
6.5 Corundum crucible.
7 Sampling and specimen preparation
7.1 Laboratory specimen
Sampling and specimen preparation shall be carried out, in accordance with GB/T
10322.1. Generally, the specimen particle size is 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.
The requirements for high combined water and easy oxidation content are in accordance
with GB/T 6730.1.
7.2 Preparation of pre-dried specimens
Thoroughly mix the laboratory specimens. Take samples using the increment specimen
reduction method. According to the provisions of GB/T 6730.1, dry the specimen at a
temperature of 105 °C ± 2 °C. Cool it to room temperature in a desiccator for later use.
8 Analytical procedures
8.1 Number of measurements
According to Appendix B, the same pre-dried specimen shall be measured
independently at least twice.
Note: "Independent" means that the results of the second and subsequent measurements are not
affected by the results of the previous measurements. In this analytical method, this condition
means that the same measured object is independently and repeatedly measured, in a short
period of time, by the same operator, using the same equipment and the same test method, in
the same laboratory, including the use of appropriate recalibration.
8.2 Specimen size
Weigh approximately 0.50 g of the pre-dried specimen (see 7.2), accurate to 0.0001 g.
The specimen weighing operation shall be carried out as quickly as possible, to prevent
the specimen from absorbing moisture again.
8.3 Blank test and verification test
8.3.1 Blank test
Carry out a blank test, along with the specimen analysis. All reagents shall be taken
from the same reagent bottle.
8.3.2 Verification test
Along with the specimen, analyze the standard samples of the same type, for
verification tests.
8.4 Determination
8.4.1 Decomposition of specimens
Place the specimen (see 8.2) in a corundum crucible, which contains 3 g ~ 4 g of sodium
hydroxide (see 5.1) that has been pre-baked, to remove moisture. Mix evenly. Add 4 g
of sodium peroxide (see 5.2) to cover it. Place it in a muffle furnace (See 6.3). Gradually
increase the temperature from low temperature to 750 °C and melt, until red and
transparent for 5 min ~ 10 min. Shake twice in this process. Take out and cool.
8.4.2 Preparation of analytical solution
8.4.2.1 Move the cooled corundum crucible into a 400 mL beaker, which contains 100
mL of triethanolamine (see 5.13), 1 g of EDTA (see 5.3), 1 g of ascorbic acid (see 5.4),
1 g of hydroxylamine hydrochloride (see 5.5). Wait until the violent reaction stops. heat
to boiling. Remove and rinse the crucible. Boil the solution for several minutes. Cool it
slightly. Use quantitative medium-speed filter paper to filter it. Use sodium hydroxide
washing solution (see 5.12), to rinse the beaker and sediment 6 ~ 7 times. Use 5 mL of
hydrochloric acid (see 5.7), to dissolve the precipitate on the filter paper. Filter it into
the volumetric flask. After the precipitate is dissolved, use dilute hydrochloric acid (see
......
| Standard ID | GB/T 6730.84-2023 (GB/T6730.84-2023) | | Description (Translated English) | Iron ores - Determination of total rare earth content - Inductively coupled plasma atomic emission spectrometric method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | D31 | | Classification of International Standard | 73.060.10 | | Word Count Estimation | 18,188 | | Date of Issue | 2023-08-06 | | Date of Implementation | 2024-03-01 | | Drafting Organization | Baotou Rare Earth Research Institute, Baotou Customs Comprehensive Technical Service Center, Jiangsu Shagang Iron and Steel Research Institute Co., Ltd., Linyi Inspection and Certification Co., Ltd., Metallurgical Industry Information Standards Research Institute, Tianjin Baotou Rare Earth Research Institute Co., Ltd., China Northern Rare Earth (Group) High-tech Co., Ltd., Baotou Group Mining Research Institute (Limited Liability Company), Baotou Rare Earth New Material Technology R&D Center, National Tungsten and Rare Earth Product Quality Supervision and Inspection Center | | Administrative Organization | National Iron Ore and Direct Reduced Iron Standardization Technical Committee (SAC/TC 317) | | Proposing organization | China Iron and Steel Industry Association | | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Administration |
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