GB/T 18882.1-2023 English PDF (GBT18882.1-2023)

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GB/T 18882.1-2023: Chemical analysis methods of mixed rare earth oxide of ion-absorption rare earth ore - Part 1: Determination of fifteen rare earth oxides composition
GB/T 18882.1-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
CCS H 14
Replacing GB/T 18882.1-2008
Chemical analysis methods of mixed rare earth oxide of ion-
absorption rare earth ore - Part 1: Determination of fifteen
rare earth oxides composition
ISSUED ON: SEPTEMBER 07, 2023
IMPLEMENTED ON: APRIL 01, 2024
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
Introduction ... 5
1 Scope ... 6
2 Normative references ... 7
3 Terms and definitions ... 7
4 Method 1: X-ray fluorescence spectrometry ... 7
5 Method 2: Inductively coupled plasma optical emission spectroscopy ... 21
Chemical analysis methods of mixed rare earth oxide of ion-
absorption rare earth ore - Part 1: Determination of fifteen
rare earth oxides composition
Warning – Personnel using this document shall have practical experience in
formal laboratory work. This document does not address all possible security
issues. Users shall have certain professional knowledge and skills and fully realize
that improper operation may cause gas leakage, current leakage, fire or other
serious consequences.
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.
4.2.16 Lutetium oxide w (REO) ≥ 99.50%, w (Lu2O3/REO) > 99.99%, calcined at 950 ℃
for 1 h, cooled to room temperature.
4.2.17 Hydrochloric acid (ρ = 1.19 g/mL).
4.2.18 Nitric acid (ρ = 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).
4.2.22 Standard stock solution A: Weigh 0.100 0 g of cerium oxide (4.2.4) into a 100
mL beaker; use a small amount of water (4.2.1) to moisten; add 5 mL of nitric acid
(4.2.18); add 5 ~ 10 drops of hydrogen peroxide (4.2.19); heat and dissolve until clear
(if not clear, repeat the operation); add 5 mL of hydrochloric acid solution (4.2.20) and
evaporate to nearly dryness; repeat once to convert the nitrate into chloride; cool and
transfer to a 500 mL volumetric flask; use hydrochloric acid solution (4.2.21) to dilute
to the mark; mix well. This solution contains 0.2 mg of cerium oxide in 1 mL.
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
Table 3 into a 200 mL beaker; use water (4.2.1) to moisten; add 10 mL of nitric acid
(4.2.18) and 5 ~ 10 drops of hydrogen peroxide (4.2.19); heat and decompose until clear
(if not clear, repeat the operation); then, add 5 mL of hydrochloric acid solution (4.2.20)
and evaporate until nearly dry; repeat once to convert nitrate into chloride; cool and
transfer to a 250 mL volumetric flask; use hydrochloric acid solution (4.2.21) to dilute
to the mark; mix well. The content of each single rare earth oxide contained in 1 mL of
this solution is shown in Table 4.
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 ℃ for 1 h; then cool it to room temperature in a desiccator.
Follow the subsequent steps as in 4.5.3.1.
4.5.3.3 Mixed rare earth carbonate of ion-absorption rare earth ore: Place the test
material (4.5.1) in a 100 mL beaker; add 20 mL of water (4.2.1), 20 mL of hydrochloric
acid (4.2.20) and 1 mL of hydrogen peroxide (4.2.19); heat to decompose until clear;
after cooling, transfer it to a 200 mL volumetric flask; use water (4.2.1) to dilute to the
mark; mix well. Transfer 0.10 g of the test solution equivalent to the mass of rare earth
oxide into a 100 mL beaker; proceed with the subsequent steps according to 4.5.3.1.
4.5.3.4 Mixed rare earth chloride feed solution of ion-absorption rare earth ore: Transfer
the test solution (4.5.1) into a 50 mL volumetric flask; use water (4.2.1) to dilute to the
mark; mix well. Transfer 0.10 g of the feed solution (4.4.4) equivalent to the mass of
rare earth oxide into a 100 mL beaker; proceed with the subsequent steps according to
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.
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 yttrium oxide in 1 mL.
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. This solution contains 5.00 mg of lanthanum oxide in 1 mL.
5.2.22 Cerium oxide standard stock solution: Weigh 0.200 0 g of cerium oxide (5.2.4)
into a 100 mL beaker; use water (5.2.1) to moisten; add 5 mL of nitric acid (5.2.18) and
1 mL of hydrogen peroxide (5.2.19); decompose at low temperature until clear (if not
clear, repeat the operation); cool and transfer to a 100 mL volumetric flask; use water
(5.2.1) to dilute to the mark; mix well. This solution contains 2.00 mg of cerium oxide
in 1 mL.
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....