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GB/T 18882.1-2023Chemical analysis methods of mixed rare earth oxide of ion-absorption rare earth ore—Part 1:Determination of fifteen rare earth oxides composition (English PDF)

离子型稀土矿混合稀土氧化物化学分析方法 第1部分:十五个稀土元素氧化物配分量的测定

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

September 7, 2023

Implementation date

April 1, 2024

Scope

GB/T 18882.1-2023 is the English-translated version of 离子型稀土矿混合稀土氧化物化学分析方法 第1部分:十五个稀土元素氧化物配分量的测定.

GB/T 18882.1-2023 is the Chinese method for measuring how the fifteen rare earth oxides are distributed in the mixed rare earth oxides, carbonates and oxalates and in the rare earth chloride feed solutions obtained from ion-absorption rare earth ore.

It describes two methods: Method 1, X-ray fluorescence spectrometry, and Method 2, inductively coupled plasma optical emission spectrometry, each with its own measurement range; where the two ranges overlap Method 1 is recommended as the arbitration method.

It lists the reagents, the single rare earth oxide standard stock solutions and the way test materials and series standard samples are prepared. It warns that users need practical experience of formal laboratory work.

It replaces GB/T 18882.1-2008, was issued on 7 September 2023 and has applied since 1 April 2024.

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Document preview — GB/T 18882.1-2023

National Standard of the People's Republic of China

ICS
77.120.99
Classification
H 14
Replacing
GB/T 18882.1-2008

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword3
  • Introduction5
  • 1 Scope6
  • 2 Normative references7
  • 3 Terms and definitions7
  • 4 Method 1: X-ray fluorescence spectrometry7
  • 5 Method 2: Inductively coupled plasma optical emission spectroscopy21

1 Scope

This document describes the method for determining the fifteen rare earth oxides composition in mixed rare earth oxides, carbonates, oxalates, and rare earth chloride feed solutions of ion-absorption rare earth ore.

This document applies to the determination of fifteen rare earth oxides composition in mixed rare earth oxides, carbonates, oxalates, and rare earth chloride feed solutions of ion-absorption rare earth ore. It contains two methods. Method 1.X-ray fluorescence spectrometry, whose measurement range is shown in Table 1. Method 2.Inductively coupled plasma emission spectrometry, whose measurement range is shown in Table 2.

When the measurement ranges of the two methods overlap, Method 1 is recommended as the arbitration method.

4 Method 1: X-ray fluorescence spectrometry

4.2.16 Lutetium oxide w (REO) >= 99.50%, w (Lu2O3/REO) > 99.99%, calcined at 950 °C for 1 h, cooled to room temperature.

4.2.17 Hydrochloric acid (rho = 1.19 g/mL).

4.2.18 Nitric acid (rho = 1.42 g/mL).

4.2.19 Hydrogen peroxide [w (H2O2) >= 30%].

4.2.20 Hydrochloric acid solution (1+1).

4.2.21 Hydrochloric acid solution (1+19).

4.2.23 Standard stock solution B. Weigh 0.100 0 g of praseodymium oxide (4.2.5) in a 100 mL beaker; use a small amount of water (4.2.1) to moisten; add 10 mL of hydrochloric acid solution (4.2.20); heat and dissolve until clear; cool and transfer to a 200 mL volumetric flask; use hydrochloric acid solution (4.2.21) to dilute to the mark; mix well. This solution contains 0.5 mg of praseodymium oxide in 1 mL.

4.2.24 Standard stock solution C~O. Weigh each single rare earth oxide according to […]

4.5.3 Preparation of test material sample

4.5.3.1 Mixed rare earth oxide of ion-absorption rare earth ore. Place the test material (4.5.1) in a 100 mL beaker; add 5 mL of hydrochloric acid (4.2.20) [add 5 mL of nitric acid (4.2.18) for samples with high cerium content]; add 0.5 mL of hydrogen peroxide (4.2.19); heat to decompose and evaporate to near dryness. After cooling to room temperature, add 5.00 mL of scandium internal standard solution (4.2.25) or vanadium internal standard solution (4.2.26); dissolve to clear; mix well.

4.5.3.2 Mixed rare earth oxalate of ion-absorption rare earth ore. Calcine the test material (4.5.1) at 950 °C for 1 h; then cool it to room temperature in a desiccator. Follow the subsequent steps as in 4.5.3.1.

4.5.3.5 Take 0.30 mL of the solution (see 4.5.3.1 ~ 4.5.3.4); drop it evenly on the filter paper (4.2.27) spread on the glass plate; leave it for 20 min; dry it under an infrared lamp before determination.

4.5.4 Preparation of series standard samples

According to Table 6, respectively transfer the standard stock solution into 12 100 mL beakers; evaporate until almost dry; cool to room temperature; add 5.0 mL of scandium internal standard solution (4.2.25) or vanadium internal standard solution (4.2.26); dissolve to clear; mix well. Prepare standard samples according to the steps in 4.5.3.5.

The distribution values of the series standard samples are shown in Table 7.

5 Method 2: Inductively coupled plasma optical emission spectroscopy

5.2.21 Lanthanum oxide standard stock solution. Weigh 0.500 0 g of lanthanum oxide (5.2.3) into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19); heat and decompose until clear; cool and transfer to a 100 mL volumetric flask; use water (5.2.1) to dilute to the mark; mix well.

5.2.23 Praseodymium oxide standard stock solution. Weigh 0.500 0 g of praseodymium oxide (5.2.5) into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19); heat and decompose until clear; cool and transfer to a 100 mL volumetric flask; use water (5.2.1) to dilute to the mark; mix well. This solution contains 5.00 mg of praseodymium oxide in 1 mL.

5.2.27 Gadolinium oxide standard stock solution. Weigh 0.500 0 g of gadolinium oxide (5.2.9) into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19); heat and decompose until clear; cool and transfer to a 100 mL volumetric flask; use water (5.2.1) to dilute to the mark; mix well. This solution contains 5.00 mg of gadolinium oxide in 1 mL.

5.2.28 Terbium oxide standard stock solution. Weigh 0.100 0 g of terbium oxide (5.2.10) into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19); heat and decompose until clear; cool and transfer to a 100 mL volumetric flask; use water (5.2.1) to dilute to the mark; mix well. This solution contains 1.00 mg of terbium oxide in 1 mL.

5.2.31 Erbium oxide standard stock solution. Weigh 0.500 0 g of erbium oxide (5.2.13) into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19); heat and decompose until clear; cool and transfer to a 100 mL volumetric flask; use water (5.2.1) to dilute to the mark; mix well. This solution contains 5.00 mg of erbium oxide in 1 mL.

5.2.32 Thulium oxide standard stock solution. Weigh 0.100 0 g of thulium oxide (5.2.14) into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19); heat and decompose until clear; cool and transfer to a 100 mL volumetric flask; use water (5.2.1) to dilute to the mark; mix well. This solution contains 1.00 mg of thulium oxide in 1 mL.

5.2.33 Ytterbium oxide standard stock solution. Weigh 0.500 0 g of ytterbium oxide (5.2.15) into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19); heat and decompose until clear; cool and transfer to a 100 mL volumetric flask; use water (5.2.1) to dilute to the mark; mix well. This solution contains 5.00 mg of ytterbium oxide in 1 mL.

5.2.34 Lutetium oxide standard stock solution. Weigh 0.100 0 g of lutetium oxide (5.2.16) into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19);

5.2.35 Standard stock solutions I ~ VIII. According to Table 11, weigh each single rare earth oxide (see 5.2.2 ~ 5.2.16) into a 200 mL beaker; use water (5.2.1) to moisten; add 10 mL of hydrochloric acid (5.2.17) and 1 mL of hydrogen peroxide (5.2.19); […]

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 21 pages — is available in the English PDF.

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Editions of GB/T 18882.1

EditionTitleRevisionStatus
GB/T 18882.1-2023Chemical analysis methods of mixed rare earth oxide of ion-absorption rare earth ore—Part 1:Determination of fifteen rare earth oxides compositioncurrent editionCurrent
GB/T 18882.1-2008Chemical analysis methods of mixed rare earth oxide of ion-absorption rare earth ore—Part 1:Determination of fifteen rare earth oxides compositionprevious editionSuperseded

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