GB/T 18882.1-2008 English PDF (GBT18882.1-2008)

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GB/T 18882.1-2008: Chemical analysis methods of mixed rare earth oxide of ion-absorbed type RE ore -- Determination of fifteen REO relative content
GB/T 18882.1-2008
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 14
Replacing GB/T 18882.2~18882.3-2002
Chemical analysis methods of mixed rare earth oxide
of ion-absorbed type RE ore - Determination of fifteen
REO relative content
ISSUED ON. JUNE 17, 2008
IMPLEMENTED ON. DECEMBER 01, 2008
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Principle of method ... 5 
3 Reagents and materials ... 5 
4 Instruments and equipment... 7 
5 Specimen ... 7 
6 Analytical procedures ... 7 
7 Calculation and expression of analysis results... 11 
8 Precision ... 11 
9 Quality assurance and control ... 12 
10 Scope ... 13 
11 Principles of method ... 13 
12 Reagents and materials ... 13 
13 Instruments and equipment... 14 
14 Specimen ... 15 
15 Analytical procedures ... 15 
16 Calculation and expression of analytical results ... 17 
17 Precision ... 18 
18 Quality assurance and control ... 19 
Chemical analysis methods of mixed rare earth oxide
of ion-absorbed type RE ore - Determination of fifteen
REO relative content
Method 1 -- X-ray fluorescent spectrometry
1 Scope
The method specifies a method for determining the relative content of fifteen
rare earth oxides in mixed rare earth oxide of ion-absorbed type RE ore.
The method is suitable for the determination of the relative content of fifteen
rare earth oxides in mixed rare earth oxide of ion-absorbed type RE ore. (TREO
≥ 80%). The determination range (mass fraction) is. 0.20% ~ 99.00%.
2 Principle of method
The specimen is dissolved in hydrochloric acid and evaporated to near dryness,
the vanadium internal standard solution is added to prepare a thin sample.
Based on the analysis conditions, measure the X-ray fluorescence intensity
ratio of the characteristic line of the element to be measured to the characteristic
line of the internal standard element. In accordance with the linear relationship
between this ratio and the content of the element to be measured, the
corresponding mathematical model is selected to calculate the relative content
of the element to be measured.
3 Reagents and materials
3.1 Yttrium oxide (REO > 99.5%, Y2O3/REO > 99.99%).
3.2 Lanthanum oxide (REO > 99.5%, La2O3/REO > 99.99%).
3.3 Cerium oxide (REO > 99.5%, CeO2/REO > 99.99%).
3.4 Praseodymium oxide (REO > 99.5%, Pr6O11/REO > 99.99%).
3.5 Neodymium oxide (REO > 99.5%, Nd2O3/REO > 99.99%).
3.6 Samarium oxide (REO > 99.5%, Sm2O3/REO > 99.99%).
oxide.
3.23 Vanadium internal standard solution. WEIGH 15.4356 g of ammonium
metavanadate (3.19) which has been baked at 105 °C for 1 h in a 400 mL
beaker; ADD a certain amount of water, HEAT to dissolve it completely; COOL
it, TRANSFER it into a 2000 mL volumetric flask. First ADD about 1500 mL of
water, then ADD 60 mL of hydrochloric acid (3.16), USE water to dilute it to the
mark, MIX it uniformly. 1 mL of this solution contains 6.00 mg of vanadium
pentoxide.
3.24 Filter paper. Φ50 mm, fast qualitative.
3.25 P10 argon-methane gas. 10% methane + 90% argon.
4 Instruments and equipment
4.1 X-ray fluorescence spectrometer. X-ray tube power ≥ 3 kW, with a dedicated
computer.
4.2 Spectroscopic crystal. LiF200.
5 Specimen
After grinding the specimen, BAKE it in a dry box at 105 °C for 1 h, PLACE it in
a desiccator to cool it to room temperature to prepare for use.
6 Analytical procedures
6.1 Samples
WEIGH 0.1000 g of specimen (5).
6.2 Determination of quantity
WEIGH two samples (6.1), MAKE parallel measurement, TAKE the average
value.
6.3 Preparation of test pieces
PLACE the sample (6.1) in a 100 mL beaker, ADD 5 mL of hydrochloric acid
(3.20) and a little hydrogen peroxide (3.18), DISSOLVE it clearly in a low
temperature electric furnace, EVAPORATE it to near dryness; COOL it to room
temperature, then ADD 5.0 mL of vanadium internal standard solution (3.23),
DISSOLVE it clearly, MIX it uniformly. PIPETTE 0.30 mL of the test solution;
evenly DRIP it on the filter paper (3.24) which is laid flatly on the glass plate,
Method 2 -- Inductively coupled plasma atomic emission spectrometry
10 Scope
The method specifies a method for the determination of the relative content of
fifteen rare earth oxides in mixed rare earth oxide of ion-absorbed type RE ore.
The method is suitable for the determination of the relative content of fifteen
rare earth oxides in mixed rare earth oxide of ion-absorbed type RE ore. The
determination range (mass fraction) is. 0.20% to 80.00%.
11 Principles of method
The sample is decomposed by hydrochloric acid and, in a dilute hydrochloric
acid medium, directly excited by an argon plasma source, to carry out
spectrometry.
12 Reagents and materials
12.1 Yttrium oxide (REO > 99.5%, Y2O3/REO > 99.99%).
12.2 Lanthanum oxide (REO > 99.5%, La2O3/REO > 99.99%).
12.3 Cerium oxide (REO > 99.5%, CeO2/REO > 99.99%).
12.4 Praseodymium oxide (REO > 99.5%, Pr6O11/REO > 99.99%).
12.5 Neodymium oxide (REO > 99.5%, Nd2O3/REO > 99.99%).
12.6 Samarium oxide (REO > 99.5%, Sm2O3/REO > 99.99%).
12.7 Europium oxide (REO > 99.5%, Eu2O3/REO > 99.99%).
12.8 Gadolinium oxide (REO > 99.5%, Gd2O3/REO > 99.99%).
12.9 Terbium oxide (REO > 99.5%, Tb4O7/REO > 99.99%).
12.10 Dysprosium oxide (REO > 99.5%, Dy2O3/REO > 99.99%).
12.11 Holmium oxide (REO > 99.5%, Ho2O3/REO > 99.99%).
12.12 Erbium oxide (REO > 99.5%, Er2O3/REO > 99.99%).
12.13 Thulium oxide (REO > 99.5%, Tm2O3/REO > 99.99%).
12.14 Ytterbium oxide (REO > 99.5%, Yb2O3/REO > 99.99%).
14 Specimen
After grinding the specimen, BAKE it in a dry box at 105 °C for 1 h, PLACE it in
a desiccator, COOL it to room temperature, WEIGH it.
15 Analytical procedures
15.1 Samples
WEIGH 0.3000 g of the specimen (14).
15.2 Determination quantity
PERFORM independently two determinations, TAKE the average value.
15.3 Preparation of analytical test solution
15.3.1 PLACE the sample (15.1) in a 100 mL beaker, ADD 20 mL of hydrochloric
acid (12.17) and 0.5 mL of hydrogen peroxide (12.16) (when the Ce content is
high, add more hydrogen peroxide or otherwise use nitric acid to treat it), HEAT
to dissolve it until big bubbles appear and are clear; COOL it, TRANSFER it into
a 100 mL volumetric flask, USE water to dilute it to the mark, MIX it uniformly.
15.3.2 PIPETTE 10.00 mL of the above test solution (15.3.1) into a 100 mL
volumetric flask, ADD another 8 mL of hydrochloric acid (12.17), USE water to
dilute it to the mark, MIX it uniformly to prepare for determination.
15.4 Preparation of standard solution
In accordance with Table 7, respectively PIPETTE the corresponding volume of
the mixed standard stock solution of rare earth oxide (12.19) into a 200 mL
volumetric flask, ADD 18 mL of hydrochloric acid (12.17), USE water to dilute it
to the mark, MIX it uniformly. 1 mL of this standard solution contains 0.3 mg of
rare earth oxide. The relative content of each rare earth oxide is as shown in
Table 8.
Table 7
No. of standard solution
Pipetted mixed standard stock solution of rare earth oxide/mL
7# high-yttrium type
8# high-yttrium type
9# high-yttrium type
10# high-yttrium type
11# high-yttrium type